CN104624180A - Preparation method of low-dimension bismuth titanate system nano material on titanium substrate with visible light response - Google Patents

Preparation method of low-dimension bismuth titanate system nano material on titanium substrate with visible light response Download PDF

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CN104624180A
CN104624180A CN201510071679.8A CN201510071679A CN104624180A CN 104624180 A CN104624180 A CN 104624180A CN 201510071679 A CN201510071679 A CN 201510071679A CN 104624180 A CN104624180 A CN 104624180A
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preparation
titanium substrate
visible light
low
nano material
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刘晓芳
陶柱
龚婷
周思全
范永康
孙华君
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Wuhan University of Technology WUT
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Wuhan University of Technology WUT
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Abstract

The invention relates to a preparation method of a low-dimension bismuth titanate system nano material on titanium substrate with visible light response. The preparation method comprises the steps of (1) preparing a precursor, namely preparing mixed solution of titanium source and bismuth titanate, adjusting pH (potential of hydrogen), mixing magnetically and extracting and filtering; (2) preparing powder, namely adding a mineralizing agent into a reaction kettle, transferring the extracted and filtered sample obtained in the step (1) into the reaction kettle, adding a pre-processed titanium substrate, sealing the reaction kettle, heating to carry out a hydrothermal reaction; and (3) cooling to room temperature, taking out the sample, rinsing, and drying, so as to obtain the low-dimension Bi4Ti3O12 powdered material. The preparation method has the advantages that the prepared catalyst has relatively narrow forbidden bandwidth, can use visible light and has high reaction activity; the excellent conductivity is guaranteed by the Ohm contact between the titanium substrate and a semiconductor, the prepared catalyst can degrade methyl orange effectively under the irradiation of ultraviolet light or visible light, and the catalyst is suitable for large-scale preparation.

Description

There is the preparation method of low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate
Technical field
The present invention relates to Hydrothermal Synthesis catalysis material in titanium substrate, particularly a kind of preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate.
Background technology
Environmental pollution and energy shortage are 21 century facing mankinds and significant problem urgently to be resolved hurrily, the switch technology researching and developing novel fungible energy source and the high-efficiency cleaning energy is extremely urgent, photocatalysis is using its room temperature deep reaction and can directly utilize solar energy to drive the special performances such as reaction as light source, and becomes a kind of desirable environmental pollution treatment technology and clear energy sources production technology.
TiO 2the studied and maximum semiconductor light-catalyst of application at present, but TiO 2intrinsic defect limits practical application in industry and the development of photocatalysis technology, and as on the low side in photo-quantum efficiency, spectral response range is narrow.Around the solution of these problems, development plays two Disciplinary Frontiers of Photocatalitic Technique of Semiconductor research: 1, to TiO 2carry out modification, to expand its effective light frequency response range, improve the utilization ratio of sunshine, improve its photocatalytic activity; 2, development of new semiconductor light-catalyst, requires that it has obvious response to visible ray, and has high photocatalytic activity.
Bismuth titanates (Bi 4ti 3o 12) there is cheapness, nontoxic and advantages of environment protection, be a kind of material being applied to super tool potentiality in photocatalysis.At present, bismuth titanates (Bi 4ti 3o 12) preparation method a lot, as sol-gel process, electrochemical deposition method, electrophoretic deposition, vacuum vapor deposition method etc.Above-mentioned correlation technique has all successfully prepared bismuth titanates (Bi 4ti 3o 12) material, its Bi prepared 4ti 3o 12basic based on powder, although easy to use, and specific area is comparatively large, and photocatalysis performance is higher, the Bi suspended 4ti 3o 12be difficult to separate recovery after catalysis terminates from the aqueous solution, thus need to carry out immobilized process to it.Therefore, explore hydro-thermal in titanium substrate and prepare bismuth titanates (Bi 4ti 3o 12) research of material is very significant.
Summary of the invention
The object of the invention is the deficiency overcoming prior art difficult separation and recycling, there is provided a kind of in titanium substrate Hydrothermal Synthesis there is the method for visible light-responded low-dimensional bismuth titanates system nano material, to obtain the material being used as visible light catalytic aspect, this kind of material has that cost is low, catalyst recoverable, preparation method is simple, is easy to the advantages such as suitability for industrialized production.
The present invention solves the problems of the technologies described above adopted technical scheme, has the preparation method of low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate, includes following steps:
1) preparation of presoma: the mixed solution of configuration titanium source and bismuth nitrate, adjust ph, suction filtration after magnetic agitation;
2) preparation of powder: add mineralizer in reactor, and transfer step 1) in sample after suction filtration in reactor, add the titanium substrate that pretreatment is good, after reactor sealing, heating is to carry out hydro-thermal reaction;
3) be cooled to room temperature, take out sample, through washing, after drying, obtain low-dimensional Bi 4ti 3o 12powder body material.
By such scheme, step 1) described in mixed solution in also include Pr (NO 3) 36H 2o, La (NO 3) 36H 2o or Nd (NO 3) 36H 2o.
By such scheme, described hydrothermal temperature is 180 ~ 220 DEG C, is incubated 6 ~ 48 hours.
By such scheme, step 1) described in pH value 10-14.
By such scheme, described mineralizer is NaOH, potassium hydroxide or lithium hydroxide.
By such scheme, described titanium source is butyl titanate, isopropyl titanate, TiF 4, TiCl 4, Ti (SO 4) 2or TiO 2.
By such scheme, described titanium substrate pretreatment method: adopt sand papering, cleaned by the mixed solution that red fuming nitric acid (RFNA), ammonium fluoride and urea are put in titanium substrate, then deionization washing, washes of absolute alcohol, is finally placed in absolute ethyl alcohol sealing and preserves.
By such scheme, described titanium substrate is titanium sheet or titanium wire network.
By such scheme, described has low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate, and its chemical formula is Bi 4-xa xti 3o 12, wherein A=La, Pr or Nd, x=0 ~ 1.5.
The present invention selects titanium as matrix, and it has good electric conductivity, corrosion resistance and better mechanical strength, and titanium may participate in Bi in the mode of ion under the condition of HTHP 4ti 3o 12synthetic reaction.The institutional framework of bismuth titanates system nano material changes with preparation condition and changes, and all has good photocatalysis performance.The bismuth titanates system growth course of microcosmic defers to Ostwald ripening mechanisms, is divided into dissolving, nucleation and crystal growth three phases.At the hydro-thermal reaction initial stage, being first that the surface of titanium source added etc. and titanium sheet is dissolved gradually in the environment of 180 DEG C of-240 DEG C of molten caustic sodas, is Bi 4ti 3o 12the growth of nanocrystal provides titanium source, and predecessor Bi and Ti is with unformed Bi 2o 3nH 2o and TiO 2nH 2the sedimentary form of O is evenly dispersed in the mineralizer aqueous solution.Under higher reaction temperature and crystallization time, in order to reduce free surface energy Bi 2o 3nH 2o and TiO 2nH 2o mutually can adsorb and form reunion; Along with the prolongation of crystallization time, Bi 2o 3nH 2o and TiO 2nH 2o constantly dissolves under high mineralizer concentration, and constitution water and hydroxyl are sloughed in collision mutually, are promptly converted into the Bi that free energy is lower 4ti 3o 12crystalline phase, the nucleation and crystallization of bismuth titanates is that each aggregate directly carries out.Bismuth titanates crystal grain is along with the prolongation of crystallization time, and the little crystal grain of a part just crystallization is unstable, more again dissolves, due to Ti a large amount of in now solution 4+, Bi 3+, OH -the hydrogen-oxygen group of ion cluster and non-bridging structure, under such circumstances, ion in the continuous absorbent solution of bismuth titanates crystal grain of first nucleation and growth process and ion cluster are grown up, spontaneous at titanium substrate surface formation nano wire or nanometer sheet low-dimensional nano structure under high-temperature high-voltage reaction condition subsequently.
The invention has the advantages that: titanium substrate (titanium sheet and titanium wire network) surface after treatment forms the attachment difficult drop-off that plurality of grooves is beneficial to catalyst; Titanium substrate (titanium sheet and titanium wire network) has good electric conductivity, corrosion resistance and better mechanical strength, is easy to the immobilized of catalyst and recycles; Obtained catalyst has the energy gap of relative narrower, can utilize visible ray, have higher reactivity; Ohmic contact between titanium substrate and semiconductor ensure that good electric conductivity, and obtained catalyst all can effectively be degraded methyl orange under ultraviolet light or radiation of visible light, can scale preparation.
Gained bismuth titanates (Bi of the present invention 4ti 3o 12) material thickness is between hundreds of nanometer is to tens microns, and its institutional framework is controlled.By changing synthesis condition, the institutional framework of film product is changed to nano wire by nanometer sheet.
Accompanying drawing explanation
Fig. 1 is the bismuth titanates (Bi that the embodiment of the present invention 1,2,3 obtains 4ti 3o 12) XRD collection of illustrative plates;
Fig. 2 is the bismuth titanates (Bi that the embodiment of the present invention 1 obtains 4ti 3o 12) SEM picture;
Fig. 3 is the bismuth titanates (Bi that the embodiment of the present invention 1 obtains 4ti 3o 12) TEM picture;
Fig. 4 is the bismuth titanates (Bi that the embodiment of the present invention 1 obtains 4ti 3o 12) light-catalyzed reaction medium ultraviolet-visible absorption curvilinear motion;
Fig. 5 is the bismuth titanates (Bi that the embodiment of the present invention 1 obtains 4ti 3o 12) UV-vis collection of illustrative plates;
Bismuth titanates (the Bi that under Fig. 6 Hg lamp irradiation, embodiment 1 is obtained 4ti 3o 12) removal to methyl orange.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention is described further.
Embodiment 1 preparation of bismuth titanates (in the titanium sheet)
Adopt analytically pure Bi (NO 3) 35H 2o, Ti (SO 4) 2for raw material, NaOH solution is mineralizer, titanium sheet substrate pretreatment method: adopt sand papering, the mixed solution that red fuming nitric acid (RFNA), ammonium fluoride and urea are put in titanium substrate is cleaned, then deionization washing, washes of absolute alcohol, is finally placed in absolute ethyl alcohol sealing and preserves.First titanium sulfate and bismuth nitrate are dissolved in deionized water in the ratio of 1.5:4 (mol ratio), stir and make to mix.Add NaOH and regulate its pH to 13, magnetic agitation solution obtains predecessor to the completely rear washing of precipitation.Using the NaOH solution of 35ml (compactedness 70%) 0.5mol/L as mineralizer, predecessor being transferred to 50ml is in the stainless steel cauldron of liner with polytetrafluoroethylene (PTFE), adds the titanium sheet of anticipating, is sealed by reactor.Reactor is heated to 220 DEG C, is incubated 24h at this temperature, take out after being cooled to room temperature, washing, dry obtained bismuth titanates (Bi 4ti 3o 12) film sample.
Embodiment 2 preparation of La doped bismuth titanate (in the titanium sheet)
Adopt analytically pure Bi (NO 3) 35H 2o, TiCl 4, La (NO 3) 36H 2o is raw material, and NaOH solution is mineralizer, and titanium sheet substrate pretreatment method is with embodiment 1.First bismuth nitrate, titanium tetrachloride and the lanthanum nitrate ratio in 4:3.25:0.75 (mol ratio) is dissolved in deionized water, stir and make to mix.Add NaOH and regulate its pH to 13, magnetic agitation solution obtains predecessor to the completely rear washing of precipitation.Using the NaOH solution of 35ml (compactedness 70%) 12.0mol/L as mineralizer, predecessor being transferred to 50ml is in the stainless steel cauldron of liner with polytetrafluoroethylene (PTFE), adds the titanium sheet of anticipating, is sealed by reactor.Reactor is heated to 220 DEG C, is incubated 16h at this temperature, take out after being cooled to room temperature, washing, dry obtained La doped bismuth titanate (Bi 3.25pr 0.75ti 3o 12) film sample.
Embodiment 3 preparation of bismuth titanates (on the titanium wire network)
Adopt analytically pure Bi (NO 3) 35H 2o, TiCl 4for raw material, NaOH solution is mineralizer, and titanium wire network substrate pretreatment method is with embodiment 1.First titanium tetrachloride and bismuth nitrate are dissolved in deionized water in the ratio of 2:4 (mol ratio), stir and make to mix.Add NaOH and regulate its pH to 13, magnetic agitation solution is to the completely rear washing of precipitation.Using the NaOH solution of 30ml (compactedness 60%) 7mol/L as mineralizer, predecessor being transferred to 50ml is in the stainless steel cauldron of liner with polytetrafluoroethylene (PTFE), adds the 50 order titanium wire networks of anticipating, is sealed by reactor.Reactor is heated to 180 DEG C, is incubated 36h at this temperature, take out after being cooled to room temperature, washing, dry obtained bismuth titanates (Bi 4ti 3o 12) film sample.
Instrument detects to be analyzed:
Detected by XRD, SEM, TEM, UV, UV-vis, the testing result of above-mentioned example products therefrom is shown in accompanying drawing 1 ~ 6.As we know from the figure, the method has prepared the higher Bi of degree of crystallinity 4ti 3o 12, and confirm that this material has the potentiality of photocatalysis degradation organic contaminant.
Fig. 1 is the bismuth titanates (Bi that embodiment 1,2,3 obtains 4ti 3o 12) the XRD collection of illustrative plates of film.As seen from the figure, diffraction maximum is relatively more sharp-pointed, shows Bi 4ti 3o 12crystallization is complete, basically identical with JCP-DS (NO.35-0795) standard spectrum, shows that synthetic product is the BTO of orthorhombic phase perovskite structure, and does not exist any miscellaneous.Lattice paprmeter a=5.437 can be calculated, b=32.379, c=5.475 by Tu Zhong three strongest ones line corresponding crystal face (171) (200) (111).
Fig. 2 is the bismuth titanates (Bi that embodiment 1 obtains 4ti 3o 12) the SEM picture of film.Result shows that the basic pattern of bismuth titanates is nanometer sheet, and there is nano wire in the surrounding of sheet also length, and nanometer sheet is square substantially, and the length of side is about 5 μm, and the length of nano wire is less than 10 μm.Fig. 3 is the bismuth titanates (Bi that embodiment 1 obtains 4ti 3o 12) the TEM picture of film.The length demonstrating nano wire is further about about 2 μm, and width is about 70nm, and corresponding interplanar distance is 0.408nm.Fig. 4 is the bismuth titanates (Bi that embodiment 1 obtains 4ti 3o 12) the UV-Visible absorption curvilinear motion of methyl orange in light-catalyzed reaction, the maximum absorption wavelength λ of bismuth titanates as seen from the figure gabout 463nm, consistent with bibliographical information.Fig. 5 is the UV, visible light DRS of the bismuth titanates sample that embodiment 1 obtains.The absorbing wavelength λ of bismuth titanates gabout 463nm, according to formula: as E g(eV)=1240/ λ g(nm), Bi 4ti 3o 12band gap calculation be about 2.55eV, be starkly lower than TiO 2energy gap 3.2eV.Fig. 6 is the bismuth titanates (Bi that under Hg lamp irradiation, embodiment 1 is obtained 4ti 3o 12) removal to methyl orange.This experiment with 500W mercury lamp for light source, power remains unchanged, catalyst amount is 0.2g/100mL, methyl orange initial concentration is 10mg/L, by this concentration 200ml methyl orange solution and catalyst fines in the dark stirring and adsorbing 30 minutes before reaction, make dyestuff, catalyst reach adsorption-desorption balance, then open light source carry out photocatalytic degradation reaction.Methyl orange is a kind of persistent organic pollutants, azo formula and quinoid structure is shown respectively in acidity and alkaline solution, and azo formula and quinoid structure are the agent structures of dye composition, therefore as difficult degradation dyestuff model compound, there is certain representativeness using methyl orange.The degradation rate of methyl orange is up to 81.27% as seen from the figure, so the low-dimensional bismuth titanate nano-material inventing preparation thus can be applied in photocatalysis water treatment field.

Claims (9)

1. there is the preparation method of low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate, include following steps:
1) preparation of presoma: the mixed solution of configuration titanium source and bismuth nitrate, adjust ph, suction filtration after magnetic agitation;
2) preparation of powder: add mineralizer in reactor, and transfer step 1) in sample after suction filtration in reactor, add the titanium substrate that pretreatment is good, after reactor sealing, heating is to carry out hydro-thermal reaction;
3) be cooled to room temperature, take out sample, through washing, after drying, obtain low-dimensional Bi 4ti 3o 12powder body material.
2. the preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate according to claim 1, is characterized in that step 1) described in mixed solution in also include Pr (NO 3) 36H 2o, La (NO 3) 36H 2o or Nd (NO 3) 36H 2o.
3. the preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate according to claim 1 and 2, is characterized in that described hydrothermal temperature is 180 ~ 220 DEG C, is incubated 6 ~ 48 hours.
4. the preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate according to claim 1 and 2, is characterized in that step 1) described in pH value 10-14.
5. the preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate according to claim 1 and 2, is characterized in that described mineralizer is NaOH, potassium hydroxide or lithium hydroxide.
6. the preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate according to claim 1 and 2, is characterized in that described titanium source is butyl titanate, isopropyl titanate, TiF 4, TiCl 4, Ti (SO 4) 2or TiO 2.
7. the preparation method with low-dimensional bismuth titanate nano-material in visible light-responded titanium substrate according to claim 1 and 2, it is characterized in that described titanium substrate pretreatment method: adopt sand papering, the mixed solution that red fuming nitric acid (RFNA), ammonium fluoride and urea are put in titanium substrate is cleaned, then deionization washing, washes of absolute alcohol, is finally placed in absolute ethyl alcohol sealing and preserves.
8. the preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate according to claim 7, is characterized in that described titanium substrate is titanium sheet or titanium wire network.
9. the preparation method with low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate according to claim 1 and 2, it is characterized in that described having low-dimensional bismuth titanates system nano material in visible light-responded titanium substrate, its chemical formula is Bi 4-xa xti 3o 12, wherein A=La, Pr or Nd, x=0 ~ 1.5.
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CN114653358A (en) * 2022-05-07 2022-06-24 桂林电子科技大学 Bi3.25La0.75Ti3O12Application of nanowires in degradation of dichlorophenol in wastewater

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