CN103523824A - Preparation method of nano flaky ferroelectric material for photocatalysis - Google Patents
Preparation method of nano flaky ferroelectric material for photocatalysis Download PDFInfo
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- CN103523824A CN103523824A CN201310492111.4A CN201310492111A CN103523824A CN 103523824 A CN103523824 A CN 103523824A CN 201310492111 A CN201310492111 A CN 201310492111A CN 103523824 A CN103523824 A CN 103523824A
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Abstract
The invention relates to a preparation method of a nano flaky ferroelectric material for photocatalysis. The preparation method comprises the steps of preparing barium salt, strontium salt and titanium salt to obtain premix according to a barium strontium titanate (BaxSr1-xTiO3) molecular formula, mixing barium salt and strontium salt according to proportions and dissolving in water, adding NaOH, dissolving titanium salt in absolute ethyl alcohol, uniformly mixing the raw materials, carrying out thermal reaction for 24 hours in a high-pressure kettle at 160-200 DEG C, cooling to room temperature in air, filtering, washing and drying the mixture to obtain nano flaky barium strontium titanate powder. Compared with the prior art, the preparation method has the advantages that the process is simple and few aggregation phenomena of prepared nano particles exist; in comparison with barium strontium titanate nano powder prepared by a conventional hydrothermal method, the preparation method, which adopts butyl titanate as a titanium source, has the characteristics of high purity of a prepared sample, good crystallinity of powder and the like.
Description
Technical field
The present invention relates to the technology of preparing of flake nano ferroelectric material, especially relate to the preparation method of nano-sheet ferroelectric material for a kind of photochemical catalysis.
Background technology
Along with scientific and technological development, the industrial circle environmental pollution that especially textile industry etc. causes progressively aggravates, and water pollution has become a problem demanding prompt solution.And along with the research to governing measure, photocatalysis to degrade organic matter has progressively obtained attention because of its advantage such as efficient, inexpensive, energy-conservation.From 1972, find TiO
2since relying on luminous energy hydrogen production by water decomposition, people have produced very high interest for utilizing photocatalysis technology to administer water pollution.Through the development of many decades, existing a lot of semiconductor light-catalysts are produced out.
Yet semiconductor light-catalyst still exists three defects at present: 1, because semiconductor catalyst energy gap is larger, cause its photoresponse district in ultraviolet region, and UV-light only accounts for 4% in sunlight; 2, due to photo-generated carrier (light induced electron and photohole), in transitting to the process of catalyst surface, easily generation is compound, causes photocatalysis efficiency to decline; 3, because photocatalyst is all semi-conductors, its electroconductibility is bad, causes current carrier to be transferred to comparatively difficulty of catalyst surface.Ferroelectric material is still short at the Applicative time of photocatalysis field, but it has unique advantage and receives publicity.It is present that ferroelectric material has spontaneous polarization when lower than Curie temperature, and spontaneous polarization strength can be by external electric field oppositely.The electronegative electronics that the spontaneous separated light catalysis that is highly advantageous to of ferroelectric material produces and the hole of positively charged, be therefore expected to improve its photocatalysis efficiency in theory.
In ferroelectric material, strontium titanate (SrTiO
3) and barium titanate (BaTiO
3) itself there is good photocatalysis efficiency.Strontium titanate (SrTiO
3) and barium titanate (BaTiO
3) solid solution forms strontium-barium titanate (being BST) will increase the distortion degree of lattice, thereby allow its electronics more easily eject, to improve photocatalysis performance.It is that nano particle and good dispersion are with increase and light and reactant contact surface area that photocatalytic applications requires ferroelectric material.The method of at present synthetic BST nano-powder mainly contains sol-gel method and hydrothermal method etc.The synthetic BST powder of sol-gel method exists agglomeration comparatively serious, and the barium-strontium titanate powder degree of crystallinity that hydrothermal method synthesizes is at present poor.Aspect photocatalytic applications, catalyzer crystallinity has a huge impact the catalytic efficiency of photocatalyst.Thereby, be extremely necessary to adopt nanometer BST powder that new synthesis technique preparation has good crystallinity and good dispersity to promote it in the further application of photocatalysis field.
Summary of the invention
The problem such as the object of the invention is to solve that existing barium-strontium titanate powder synthetic technology powder granule is excessive, powder reuniting is too serious and powder crystallinity is bad, and on this basis in conjunction with the advantage of sol-gel method and traditional hydrothermal method, adopting butyl (tetra) titanate is that raw material is used hydrothermal method synthesizing flaky nano barium-strontium titanate powder.
Object of the present invention can be achieved through the following technical solutions:
A preparation method for nano-sheet ferroelectric material for photochemical catalysis, comprises the following steps:
(1) press strontium-barium titanate (Ba
xsr
1-xtiO
3) molecular formula, be x in molar ratio: (1-x): 1 configuration barium salt, strontium salt and titanium salt configuration obtain pre-composition;
(2) barium salt, strontium salt in water, are then added to NaOH, stirring and dissolving by proportioning mixed dissolution, titanium salt is dissolved in dehydrated alcohol, the ethanolic soln of titanium salt is poured in the above-mentioned aqueous solution, in constant temperature blender with magnetic force, under 600r/min condition, stirred 30min, until mix completely;
(3) mixed solution is transferred in teflon-lined autoclave, at 160-200 ℃ of insulation 24h, after reaction process finishes in air cool to room temperature, after filtration, washing, the dry nano-sheet barium-strontium titanate powder that is prepared into obtain.
In step (1), the scope of x is 0 < x < 1.
Described barium salt comprises BaCl
2, Ba (NO
3)
2or Ba (CH
3cOO)
2.
Described strontium salt comprises SrCl
2, Sr (NO
3)
2or Sr (CH
3cOO)
2.
Described titanium salt is synthetic or commercially available butyl (tetra) titanate ((C
4h
9o)
4ti).
The preferred 160-180 ℃ of temperature of reaction in step (3).
Compared with prior art, the present invention is by the advantage in conjunction with sol-gel method and traditional hydrothermal method, adopting butyl (tetra) titanate is that raw material is used hydrothermal method synthesizing flaky nano barium-strontium titanate powder, the method synthetic powder particle diameter is less, agglomeration alleviates, and synthetic powder good crystallinity and be sheet-like morphology, is expected to increase substantially its photocatalysis characteristic.Precursor liquid in above-mentioned reaction is Ti (C in above-mentioned steps (2) gained mixed solution
4h
9o)
4after hydrolysis, form complicated ions as [Ti (OH)
2.xH
2o]
2+deng, and absorption Ba
2+, Sr
2+, this ionic group generation dehydration reaction in crystallisation process, under High Temperature High Pressure, precursor dehydration comparatively fast, forms a large amount of nucleus growth, obtains strontium-barium titanate.At sol-gel method, prepare in strontium-barium titanate, butyl (tetra) titanate and barium salt, strontium salt binding form precursor, hydrolysis generates colloidal sol, and then generation gel, through calcining, generate strontium-barium titanate again, and traditional hydro-thermal rule can provide high temperature and high pressure environment, promote the hydrolysis of precursor and generate a large amount of nucleus, under control experimental temperature and the condition of time, finally obtain flake nano powder.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the strontium-barium titanate for preparing of embodiment 1;
Fig. 2 is the XRD figure of the strontium-barium titanate for preparing of embodiment 2;
Fig. 3 is the SEM figure of the strontium-barium titanate for preparing of embodiment 1;
Fig. 4 is the SEM figure of the strontium-barium titanate for preparing of embodiment 2.
Embodiment
Below by embodiment, also by reference to the accompanying drawings the present invention is further explained, but do not limit the present invention.
In embodiments of the invention, the model of major equipment used and the information of manufacturer are as follows: below by embodiment, also by reference to the accompanying drawings the present invention is further set forth, but do not limit the present invention.
In various embodiments of the present invention, the model of major equipment used and the information of manufacturer are as follows:
Ball mill: QM-2SP2 (2L), Nanjing Nan great instrument plant;
Electric heating constant-temperature blowing drying box: DHG-9240A, the grand equipment of upper Nereid company limited;
Solar simulator: PLS-SXE300C, Beijing Bo Feilai Science and Technology Ltd.;
Ultra-violet and visible spectrophotometer: UV-2550, Japanese Shimadzu.
In embodiments of the invention, the specification of raw material used and the information of manufacturer are as follows:
Embodiment 1
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.7sr
0.3tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.7:0.3:1:4; The barium salt adopting is BaCl
2.2H
2o, strontium salt is SrCl
2.2H
2o.
Weigh 1.7186g BaCl
2.2H
2o, 0.8039g SrCl
2.2H
2o, is transferred to two kinds of raw materials in Erlenmeyer flask, adds 25ml deionized water and stirring to dissolve, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.7sr
0.3tiO
3.The XRD figure and the SEM that prepare strontium-barium titanate scheme respectively as shown in figures 1 and 3.By XRD figure, can be found out, corresponding with standard diagram not neat containing other ，Qie Ge peak, assorted peak in its collection of illustrative plates, the Ba that known present method is prepared
0.7sr
0.3tiO
3for pure phase; By SEM figure, can be found out, powder reuniting phenomenon prepared by present method is lighter, and diameter of particle is less.
Embodiment 2
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.7sr
0.3tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.7:0.3:1:4; The barium salt adopting is BaCl
2.2H
2o, strontium salt is SrCl
2.2H
2o.
Weigh 1.7186g BaCl
2.2H
2o, 0.8039g SrCl
2.2H
2o, is transferred to two kinds of raw materials in Erlenmeyer flask, adds 25ml deionized water and stirring to dissolve, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.7sr
0.3tiO
3.The XRD figure and the SEM that prepare strontium-barium titanate scheme respectively as shown in Figure 2 and Figure 4.By XRD figure, can be found out, corresponding with standard diagram not neat containing other ，Qie Ge peak, assorted peak in its collection of illustrative plates, the Ba that known present method is prepared
0.7sr
0.3tiO
3for pure phase; By SEM figure, can be found out, in the form of sheets, particle diameter is in 100nm for powder granule prepared by present method.
Embodiment 3
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.7sr
0.3tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.7:0.3:1:4; The barium salt adopting is Ba (NO
3)
2, strontium salt is Sr (NO
3)
2.
Weigh 1.8295g Ba (NO
3)
2, 0.6349g Sr (NO
3)
2, two kinds of raw materials are transferred in Erlenmeyer flask, add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.7sr
0.3tiO
3.
Embodiment 4
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.7sr
0.3tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.7:0.3:1:4; The barium salt adopting is Ba (NO
3)
2, strontium salt is Sr (NO
3)
2.
Weigh 1.8295g Ba (NO
3)
2, 0.6349g Sr (NO
3)
2, two kinds of raw materials are transferred in Erlenmeyer flask, add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.7sr
0.3tiO
3.
Embodiment 5
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.3sr
0.7tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.3:0.7:1:4; The barium salt adopting is BaCl
2.2H
2o, strontium salt is SrCl
2.2H
2o.
Weigh 0.7238g BaCl
2.2H
2o, 1.8663g SrCl
2.2H
2o, is transferred to two kinds of raw materials in Erlenmeyer flask, adds 25ml deionized water and stirring to dissolve, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.3sr
0.7tiO
3.
Embodiment 6
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.3sr
0.7tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.3:0.7:1:4; The barium salt adopting is BaCl
2.2H
2o, strontium salt is SrCl
2.2H
2o.
Weigh 0.7238g BaCl
2.2H
2o, 1.8663g SrCl
2.2H
2o, is transferred to two kinds of raw materials in Erlenmeyer flask, adds 25ml deionized water and stirring to dissolve, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.3sr
0.7tiO
3.
Embodiment 7
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.3sr
0.7tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.3:0.7:1:4; The barium salt adopting is Ba (NO
3)
2, described strontium salt is Sr (NO
3)
2.
Weigh 0.7841g Ba (NO
3)
2, 1.4814g Sr (NO
3)
2, two kinds of raw materials are transferred in Erlenmeyer flask, add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.3sr
0.7tiO
3.
Embodiment 8
Photochemical catalysis is a preparation method for strontium-barium titanate with nano-sheet ferroelectric material, with Ba
0.3sr
0.7tiO
3for example, calculate in molar ratio, wherein the barium in barium salt: the strontium in strontium salt: the titanium in butyl (tetra) titanate: sodium hydroxide is 0.3:0.7:1:4; The barium salt adopting is Ba (NO
3)
2, described strontium salt is Sr (NO
3)
2.
Weigh 0.7841g Ba (NO
3)
2, 1.4814g Sr (NO
3)
2, two kinds of raw materials are transferred in Erlenmeyer flask, add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms strong alkali environment.
Utilize graduated cylinder to get 3.4ml butyl (tetra) titanate, add appropriate dehydrated alcohol to form the ethanolic soln of butyl (tetra) titanate, this ethanolic soln is poured in above-mentioned Erlenmeyer flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stir 30min, afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 ℃, carry out hydro-thermal reaction, time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtain ferroelectric material strontium-barium titanate Ba
0.3sr
0.7tiO
3.
Claims (6)
1. a preparation method for nano-sheet ferroelectric material for photochemical catalysis, is characterized in that, the method comprises the following steps:
(1) press strontium-barium titanate (Ba
xsr
1-xtiO
3) molecular formula, be x in molar ratio: (1-x): 1 configuration barium salt, strontium salt and titanium salt configuration obtain pre-composition;
(2) barium salt, strontium salt in water, are then added to NaOH, stirring and dissolving by proportioning mixed dissolution, titanium salt is dissolved in dehydrated alcohol, the ethanolic soln of titanium salt is poured in the above-mentioned aqueous solution, in constant temperature blender with magnetic force, under 600r/min condition, stirred 30min, until mix completely;
(3) mixed solution is transferred in teflon-lined autoclave, at 160-200 ℃ of insulation reaction 24h, after reaction process finishes in air cool to room temperature, after filtration, washing, the dry nano-sheet barium-strontium titanate powder that is prepared into obtain.
2. the preparation method of nano-sheet ferroelectric material for a kind of photochemical catalysis according to claim 1, is characterized in that, in step (1), the scope of x is 0 < x < 1.
3. the preparation method of nano-sheet ferroelectric material for a kind of photochemical catalysis according to claim 1 and 2, is characterized in that, described barium salt comprises BaCl
2, Ba (NO
3)
2or Ba (CH
3cOO)
2.
4. the preparation method of nano-sheet ferroelectric material for a kind of photochemical catalysis according to claim 1 and 2, is characterized in that, described strontium salt comprises SrCl
2, Sr (NO
3)
2or Sr (CH
3cOO)
2.
5. the preparation method of nano-sheet ferroelectric material for a kind of photochemical catalysis according to claim 1 and 2, is characterized in that, described titanium salt is synthetic or commercially available butyl (tetra) titanate ((C
4h
9o)
4ti).
6. the preparation method of nano-sheet ferroelectric material for a kind of photochemical catalysis according to claim 1, is characterized in that the preferred 160-180 ℃ of temperature of reaction in step (3).
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| CN106757351A (en) * | 2016-11-18 | 2017-05-31 | 西南石油大学 | A kind of preparation method of barium strontium titanate crystal beam material |
| CN108355683A (en) * | 2018-04-03 | 2018-08-03 | 哈尔滨理工大学 | A kind of bismuth oxybromide/barium strontium titanate preparation method and application |
| CN108465464A (en) * | 2018-04-02 | 2018-08-31 | 哈尔滨理工大学 | A kind of preparation method and application of barium strontium titanate/pucherite |
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| CN106757351A (en) * | 2016-11-18 | 2017-05-31 | 西南石油大学 | A kind of preparation method of barium strontium titanate crystal beam material |
| CN108465464A (en) * | 2018-04-02 | 2018-08-31 | 哈尔滨理工大学 | A kind of preparation method and application of barium strontium titanate/pucherite |
| CN108465464B (en) * | 2018-04-02 | 2021-03-23 | 哈尔滨理工大学 | Preparation method and application of barium strontium titanate/bismuth vanadate |
| CN108355683A (en) * | 2018-04-03 | 2018-08-03 | 哈尔滨理工大学 | A kind of bismuth oxybromide/barium strontium titanate preparation method and application |
| CN108906079A (en) * | 2018-06-27 | 2018-11-30 | 中国科学技术大学 | A kind of photocatalytic system, preparation method and application |
| CN108906079B (en) * | 2018-06-27 | 2020-10-27 | 中国科学技术大学 | Photocatalytic system, preparation method and application thereof |
| CN109759047A (en) * | 2019-03-20 | 2019-05-17 | 南京工业大学 | Preparation method of barium strontium titanate aerogel photocatalyst |
| CN110090652A (en) * | 2019-05-07 | 2019-08-06 | 重庆大学 | A method of it preparing chlorine four and aoxidizes three bismuths/strontium ferrite composite magnetic catalysis material |
| CN113600169A (en) * | 2021-06-08 | 2021-11-05 | 电子科技大学长三角研究院(湖州) | Solid solution photocatalyst for photocatalytic oxidation degradation of toluene and preparation method thereof |
| CN114505068A (en) * | 2022-03-03 | 2022-05-17 | 中山大学 | Piezoelectric catalyst and preparation method and application thereof |
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