CN103523824B - The preparation method of nano-sheet ferroelectric material for a kind of photocatalysis - Google Patents
The preparation method of nano-sheet ferroelectric material for a kind of photocatalysis Download PDFInfo
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Abstract
The present invention relates to the preparation method of a kind of photocatalysis nano-sheet ferroelectric material, by barium strontium titanate (BaxSr1-xTiO3) molecular formula, configuration barium salt, strontium salt and titanium salt configuration obtain pre-composition, barium salt, strontium salt by proportioning mixed dissolution in water and add NaOH, titanium salt is dissolved in absolute ethyl alcohol, after above-mentioned raw materials mixes in autoclave in 160-200 DEG C of insulation reaction 24h, then cool to room temperature in air, after filtration, washing, the dry nano-sheet barium-strontium titanate powder that is prepared into obtain. Compared with prior art, preparation technology of the present invention is simple, and preparation nanoparticle agglomerates phenomenon is few; Compared with preparing barium strontium titanate nano powder with traditional hydro-thermal method, it is titanium source that the present invention adopts butyl titanate, the feature such as high and powder good crystallinity of prepared sample purity.
Description
Technical field
The present invention relates to the technology of preparing of flake nano ferroelectric material, especially relate to a kind of photocatalysis nanometer sheetThe preparation method of shape ferroelectric material.
Background technology
Along with scientific and technological development, the industrial circle environmental pollution that especially textile industry etc. causes progressively aggravates, waterBody pollution has become a problem demanding prompt solution. And along with the research to governing measure, photocatalytic degradation is organicThing has progressively obtained attention because of its advantage such as efficient, inexpensive, energy-conservation. Found TiO from 19722Can rely on luminous energySince hydrogen production by water decomposition, people have produced very high interest for utilizing photocatalysis technology to administer water pollution. Through numberThe development of 10 years, existing a lot of semiconductor light-catalysts are produced out.
But semiconductor light-catalyst still exists three defects at present: 1, because semiconductor catalyst forbidden band is wideSpend greatlyr, cause its photoresponse district in ultraviolet region, and ultraviolet light only accounts for 4% in sunshine; 2, due toPhoto-generated carrier (light induced electron and photohole) easily occurs compound in the process that transits to catalyst surface, leadsCausing photocatalysis efficiency declines; 3, because photochemical catalyst is all semiconductors, its electric conductivity is bad, causes carrier to turnMove to comparatively difficulty of catalyst surface. Ferroelectric material is still short at the Applicative time of photocatalysis field, but it has uniquenessAdvantage and receive publicity. It is present that ferroelectric material has spontaneous polarization when lower than Curie temperature, and spontaneous polarizationIntensity can be by external electric field oppositely. The electronegative electricity that the spontaneous separated light catalysis that is highly advantageous to of ferroelectric material producesThe hole of son and positively charged, is therefore expected to improve its photocatalysis efficiency in theory.
In ferroelectric material, strontium titanates (SrTiO3) and barium titanate (BaTiO3) itself there is good photocatalysis efficiency.Strontium titanates (SrTiO3) and barium titanate (BaTiO3) solid solution forms barium strontium titanate (being BST) will increase lattice abnormalRange degree, thus allow its electronics more easily eject, to improve photocatalysis performance. Photocatalytic applications requires ferroelectricMaterial is that nano particle and good dispersion are with increase and light and reactant contact surface area. At present synthetic BST receivesThe method of ground rice body mainly contains sol-gal process and hydro-thermal method etc. There is group in the synthetic BST powder of sol-gal processPoly-phenomenon is comparatively serious, and the barium-strontium titanate powder degree of crystallinity that hydro-thermal method synthesizes is at present poor. In photocatalytic applications sideFace, catalyst crystallinity has a huge impact the catalytic efficiency of photochemical catalyst. Thereby, be extremely necessary to adoptNew synthesis technique is prepared the nanometer BST powder with good crystallinity and good dispersion to promote it to lead in photocatalysisThe further application in territory.
Summary of the invention
The object of the invention is to solve that existing barium-strontium titanate powder synthetic technology powder granule is excessive, powder reuniting mistakeIn the problem such as serious and powder crystallinity is bad, and excellent in conjunction with sol-gal process and traditional hydro-thermal method on this basisPoint, adopting butyl titanate is that raw material uses hydro-thermal 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 photocatalysis, comprises the following steps:
(1) press barium strontium titanate (BaxSr1-xTiO3) molecular formula, be x in molar ratio: (1-x): 1 configuration barium salt, strontium saltAnd titanium salt configuration obtains pre-composition;
(2) barium salt, strontium salt in water, are then added to NaOH by proportioning mixed dissolution, stirring and dissolving, by titaniumSalt is dissolved in absolute ethyl alcohol, and the ethanolic solution of titanium salt is poured in the above-mentioned aqueous solution, in constant temperature blender with magnetic forceUnder 600r/min condition, stir 30min, until mix completely;
(3) mixed liquor is transferred in teflon-lined autoclave, at 160-200 DEG C of insulation 24h, anti-After the process of answering finishes in air cool to room temperature, after filtration, washing, the dry nano-sheet metatitanic acid that is prepared into obtainStrontium barium powder.
In step (1), the scope of x is 0 < x < 1.
Described barium salt comprises BaCl2、Ba(NO3)2Or Ba (CH3COO)2。
Described strontium salt comprises SrCl2、Sr(NO3)2Or Sr (CH3COO)2。
Described titanium salt is synthetic or commercially available butyl titanate ((C4H9O)4Ti)。
The preferred 160-180 DEG C of reaction temperature in step (3).
Compared with prior art, the present invention, by the advantage in conjunction with sol-gal process and traditional hydro-thermal method, adopts titaniumAcid butyl ester is that raw material uses hydro-thermal method synthesizing flaky nano barium-strontium titanate powder, and 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 spyProperty. Precursor liquid in above-mentioned reaction is Ti (C in above-mentioned steps (2) gained mixed liquor4H9O)4After hydrolysis, formComplicated ions is as [Ti (OH)2.xH2O]2+Deng, and absorption Ba2+、Sr2+, in crystallization process, this ion cluster occursDehydration, under HTHP, predecessor dehydration comparatively fast, forms a large amount of nucleus growth, obtains barium strontium titanate. ?Sol-gal process is prepared in barium strontium titanate, and butyl titanate and barium salt, strontium salt are in conjunction with forming predecessor, and hydrolysis generates moltenGlue, and then generate gel, then generate barium strontium titanate through calcining, and traditional hydro-thermal rule can provide high temperature and high pressure environment,Promote the hydrolysis of predecessor and generate a large amount of nucleus, under control experimental temperature and the condition of time, finally obtaining sheetNano-powder.
Brief description of the drawings
Fig. 1 is the XRD figure of the barium strontium titanate for preparing of embodiment 1;
Fig. 2 is the XRD figure of the barium strontium titanate for preparing of embodiment 2;
Fig. 3 is the SEM figure of the barium strontium titanate for preparing of embodiment 1;
Fig. 4 is the SEM figure of the barium strontium titanate for preparing of embodiment 2.
Detailed description of the invention
Also by reference to the accompanying drawings the present invention is further explained below by embodiment, but do not limit the present invention.
In embodiments of the invention, the model of capital equipment used and the information of manufacturer are as follows: below by realityExecute example and by reference to the accompanying drawings the present invention further set forth, but not limiting the present invention.
In various embodiments of the present invention, the model of capital equipment used and the information of manufacturer are as follows:
Ball mill: QM-2SP2 (2L), Nanjing Nanda Instrument Plant;
Electric heating constant-temperature blowing drying box: DHG-9240A, the grand equipment of upper Nereid Co., Ltd;
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
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.7Sr0.3TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.7:0.3:1:4; The barium salt adopting is BaCl2.2H2O, strontium salt is SrCl2.2H2O。
Weigh 1.7186gBaCl2.2H2O、0.8039gSrCl2.2H2O, is transferred to two kinds of raw materials in conical flask,Add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms by forceAlkali environment.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.7Sr0.3TiO3. Prepare the XRD figure of barium strontium titanate and SEM figure respectively asShown in Fig. 1 and Fig. 3. Can be found out by XRD figure, in its collection of illustrative plates, not contain other assorted peak and each peak and standard diagramCorresponding neat, the Ba that known this method is prepared0.7Sr0.3TiO3For pure phase; Can be found out this method by SEM figureThe powder reuniting phenomenon of preparation is lighter, and diameter of particle is less.
Embodiment 2
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.7Sr0.3TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.7:0.3:1:4; The barium salt adopting is BaCl2.2H2O, strontium salt is SrCl2.2H2O。
Weigh 1.7186gBaCl2.2H2O、0.8039gSrCl2.2H2O, is transferred to two kinds of raw materials in conical flask,Add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms by forceAlkali environment.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.7Sr0.3TiO3. Prepare the XRD figure of barium strontium titanate and SEM figure respectively asShown in Fig. 2 and Fig. 4. Can be found out by XRD figure, in its collection of illustrative plates, not contain other assorted peak and each peak and standard diagramCorresponding neat, the Ba that known this method is prepared0.7Sr0.3TiO3For pure phase; Can be found out this method by SEM figureIn the form of sheets, particle diameter is in 100nm for the powder granule of preparation.
Embodiment 3
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.7Sr0.3TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.7:0.3:1:4; The barium salt adopting is Ba (NO3)2, strontium salt is Sr (NO3)2。
Weigh 1.8295gBa (NO3)2、0.6349gSr(NO3)2, two kinds of raw materials are transferred in conical flask, add25ml deionized water and stirring is dissolved, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms highly basic ringBorder.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.7Sr0.3TiO3。
Embodiment 4
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.7Sr0.3TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.7:0.3:1:4; The barium salt adopting is Ba (NO3)2, strontium salt is Sr (NO3)2。
Weigh 1.8295gBa (NO3)2、0.6349gSr(NO3)2, two kinds of raw materials are transferred in conical flask, add25ml deionized water and stirring is dissolved, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms highly basic ringBorder.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.7Sr0.3TiO3。
Embodiment 5
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.3Sr0.7TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.3:0.7:1:4; The barium salt adopting is BaCl2.2H2O, strontium salt is SrCl2.2H2O。
Weigh 0.7238gBaCl2.2H2O、1.8663gSrCl2.2H2O, is transferred to two kinds of raw materials in conical flask,Add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms by forceAlkali environment.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.3Sr0.7TiO3。
Embodiment 6
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.3Sr0.7TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.3:0.7:1:4; The barium salt adopting is BaCl2.2H2O, strontium salt is SrCl2.2H2O。
Weigh 0.7238gBaCl2.2H2O、1.8663gSrCl2.2H2O, is transferred to two kinds of raw materials in conical flask,Add 25ml deionized water and stirring to dissolve, 1.6667gNaOH is added in above-mentioned solution, stirring and dissolving forms by forceAlkali environment.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.3Sr0.7TiO3。
Embodiment 7
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.3Sr0.7TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.3:0.7:1:4; The barium salt adopting is Ba (NO3)2, described strontium salt is Sr (NO3)2。
Weigh 0.7841gBa (NO3)2、1.4814gSr(NO3)2, two kinds of raw materials are transferred in conical flask, add25ml deionized water and stirring is dissolved, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms highly basic ringBorder.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 160 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.3Sr0.7TiO3。
Embodiment 8
Photocatalysis is a preparation method for barium strontium titanate with nano-sheet ferroelectric material, with Ba0.3Sr0.7TiO3ForExample, calculates the wherein barium in barium salt: the strontium in strontium salt: the titanium in butyl titanate: NaOH is in molar ratio0.3:0.7:1:4; The barium salt adopting is Ba (NO3)2, described strontium salt is Sr (NO3)2。
Weigh 0.7841gBa (NO3)2、1.4814gSr(NO3)2, two kinds of raw materials are transferred in conical flask, add25ml deionized water and stirring is dissolved, and 1.6667gNaOH is added in above-mentioned solution, and stirring and dissolving forms highly basic ringBorder.
Utilize graduated cylinder to get 3.4ml butyl titanate, add the ethanolic solution of appropriate absolute ethyl alcohol formation butyl titanate, willThis ethanolic solution is poured in above-mentioned conical flask, in constant temperature blender with magnetic force, under 600r/min rotating speed, stirs 30min,Afterwards suspension is transferred in teflon-lined autoclave, under the condition of 180 DEG C, carries out hydro-thermal anti-Should, the time is 24h, after hydrothermal reaction process finishes, air cooling is to room temperature, after filtration, wash, be drying to obtainFerroelectric material barium strontium titanate Ba0.3Sr0.7TiO3。
Claims (2)
1. a preparation method for nano-sheet ferroelectric material for photocatalysis, is characterized in that, the method comprise withLower step:
(1) press barium strontium titanate molecular formula BaxSr1-xTiO3, be x:(1-x in molar ratio): 1 configuration barium salt, strontium salt andTitanium salt, the scope of x is 0 < x < 1;
(2) barium salt, strontium salt in water, are then added to NaOH by proportioning mixed dissolution, stirring and dissolving, by titaniumSalt is dissolved in absolute ethyl alcohol, and the ethanolic solution of titanium salt is poured in the above-mentioned aqueous solution, in constant temperature blender with magnetic forceUnder 600r/min condition, stir 30min, until mix completely;
(3) mixed liquor is transferred in teflon-lined autoclave, at 160-200 DEG C of insulation reaction 24h,After course of reaction finishes in air cool to room temperature, after filtration, washing, the dry nano-sheet titanium that preparesAcid strontium barium powder;
Described barium salt comprises BaCl2、Ba(NO3)2Or Ba (CH3COO)2; Described strontium salt comprises SrCl2、Sr(NO3)2Or Sr (CH3COO)2; Described titanium salt is synthetic or commercially available butyl titanate ((C4H9O)4Ti)。
2. the preparation method of nano-sheet ferroelectric material for a kind of photocatalysis according to claim 1, its spyLevy and be, the preferred 160-180 DEG C of reaction temperature in step (3).
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| CN106111101B (en) * | 2016-06-23 | 2018-11-30 | 辽宁大学 | A kind of composite titanic acid barium photochemical catalyst and its preparation method and application |
| 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 |
| 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 |
| 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 | A kind of preparation method of barium strontium aerogels |
| 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 |
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