CN102002746A - Method for preparing iron oxide nano granule modified titanium dioxide nano tube array - Google Patents
Method for preparing iron oxide nano granule modified titanium dioxide nano tube array Download PDFInfo
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- CN102002746A CN102002746A CN 201010531813 CN201010531813A CN102002746A CN 102002746 A CN102002746 A CN 102002746A CN 201010531813 CN201010531813 CN 201010531813 CN 201010531813 A CN201010531813 A CN 201010531813A CN 102002746 A CN102002746 A CN 102002746A
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Abstract
The invention discloses a method for preparing an iron oxide nano granule modified titanium dioxide nano tube array, and relates to a method for preparing a titanium dioxide nano tube array. The method comprises the following steps of: pre-treating a substrate, preparing electrolyte, performing electrochemical anodic oxidation on the substrate to form an ordered titanium dioxide nano tube array film with controllable size on the surface of the substrate, treating the film in Fe(NO3)3.9H2O by ultrasonic, and taking out and drying the film after standing; and thermally treating the dried composite film layer to obtain a product. By adopting the ultrasonic and chemical deposition combined method and controlling the concentration of the Fe(NO3)3 solution, the ultrasonic time and the dipping time, iron oxide nano granules can be controllably deposited on the surface of the titanium-based titanium dioxide nano tube array and in tubes, so that the photo-catalysis efficiency of the TiO2 can be improved, the photo-response of the TiO2 can be expanded to a visible light area, the utilization rate of the sunlight is improved, and the TiO2 applied to photo-catalysis can improve the absorption capability of an electrode on visible light and the photo-catalytic degradation capability on organic pollutants.
Description
Technical field
The present invention relates to a kind of preparation method of Nano tube array of titanium dioxide, especially relate to a kind of preparation method of Nano tube array of titanium dioxide of ferric oxide nanometer particle modification.
Background technology
Environmental pollution and energy shortage are the significant problems that the 21 century mankind face and need to be resolved hurrily, and have become the important restraining factors that All-round, Coordinated and Sustainable Development is carried out by China.Carey in 1976 etc. at first propose to use titanium dioxide (TiO
2) photocatalytic degradation biphenyl and askarel, opened up TiO
2The frontier of aspect environment protection, using.Calendar year 2001 U.S. scientist Grimes etc. utilizes electrochemistry anodic oxidation to go out TiO in the Ti surface preparation
2The nano-tube array material causes people's very big concern.In recent years, synthetic caliber of several different methods and the controlled TiO of pipe range have been developed
2Nano-tube array, and it has been carried out extensive studies at aspects such as transmitter, dye sensitization solar battery, photolysis water hydrogen and opto-electronic conversion, and demonstrate tempting application prospect.Yet, TiO
2Energy gap be 3.2eV, corresponding excitation wavelength is 387nm, belongs to ultraviolet region, and is low to the effective rate of utilization of sun power a little less than the visible absorption, it is low that photoelectricity transforms quantum yield, seriously restricted its practical application.For with TiO
2The spectral response range of nano-tube array extends to visible region, thereby utilizes sunlight that it is excited efficiently, and people utilize several different methods to TiO
2The nano-tube array rete carries out modification, and for example, nonmetal doping, metal or doped metallic oxide, semi-conductor are compound etc., to strengthen its absorption to visible light.
Composite nanometer semiconductor is that two or more Nano semiconductor with different energy band structures is combined in some way, forms the composite nano material.It is wide band gap semiconducter that this recombination energy makes the narrow gap semiconductor sensitization, and wide band gap semiconducter is expanded to visible region as the photochemical reaction of photocatalyst.α-Fe
2O
3Energy gap be 2.2eV, can be by excited by visible light, though the photocatalytic activity of self is not high, and TiO
2After compound, because the difference of the two conduction band current potential can make light induced electron and hole be able to effective the separation, improve quantum yield ([1] M.R.Dhananjeyan of photocatalyst, E.Mielczarski, K.R.Thampi, Ph.Buffat, M.Bensimon, A.Kulik, J.Mielczarski, and J.Kiwi, Photodynamics and surface characterization of TiO
2And Fe
2O
3Photocatalysts immobilized on modified polyethylene films.J.Phys.Chem.B, 2001,105:12046-12055; [2] Li Xiuying, Wang Jingyu, Wang Xiaoyu, etc., Fe
2O
3-TiO
2The preparation of magnetic composite and visible light catalytic performance. SCI, 2001,4:662-666.).Yet, with Fe
2O
3Nano material is compound to TiO
2Report on the nano-tube array rete seldom.In recent years, ([3] S.K.Mohapatra, S.Banerjee, M.Misra, Synthesis of Fe such as Misra
2O
3/ TiO
2Nanorod-nanotube arrays by filling TiO
2Nanotubea with Fe.Nanotechnology, 2008,19:315601) adopt the pulse electrodeposition method that Fe is filled in TiO
2Synthesized Fe in the nanotube
2O
3/ TiO
2Nanometer rod-nano-tube array, this composite array has stronger visible absorption because of the filling of Fe.([4] A.I.Kontos, V.Likodimos, T.Stergiopoulos such as Falas, D.S.Tsoukleris, P.Falaras, I.Rabias, G.Papavassiliou, D.Kim, J.Kunze, P.Schmuk, Chem.Mater., 2009,21:662-672) the synthetic ferric oxide nanometer particle is deposited on TiO
2Obtained the TiO of ferric oxide nanometer particle functionalization in the nanotube
2The degraded to organic pollutant under ultraviolet lighting of nano-tube array, this material demonstrates higher photocatalytic activity.([5] S.Y.Kuang, L.X.Yang, S.L.Luo, Q.Y.Cai, Fabrication, characterization and photoelectrochemical properties of Fe such as Cai
2O
3Modified TiO
2Nanotube arrays.Appl.Surf.Sci., 2009,255:7385-7388) adopt chemical bath deposition method with TiO
2Nano-tube array is at FeCl
3, H
2O, NaOH, and H
2Circulate successively in the O solution and flood, obtained Fe
2O
3The TiO that modifies
2Nano-tube array demonstrates and is better than pure TiO
2The photoelectrochemical behaviour of nano-tube array.Yet the method for preparing complex process is unfavorable for realizing suitability for industrialized production.
Summary of the invention
It is a kind of simple to operate that purpose of the present invention is intended to provide, and is easy to realize the preparation method of the Nano tube array of titanium dioxide that the ferric oxide nanometer particle of suitability for industrialized production is modified.
The present invention includes following steps:
1) with the substrate material surface cleaning pretreatment, prepare electrolytic solution then, electrochemical anodic oxidation is carried out in substrate, can construct one deck at substrate surface and arrange film of Nano tube array of titanium dioxide orderly, controllable size;
In step 1), described base material can be pure titanium material; Described cleaning surfaces pre-treatment can adopt acetone, second alcohol and water that substrate material surface is carried out ultrasonic cleaning successively; Described electrolytic solution can be the aqueous solution of 0.1～1.5wt%HF, and the described condition that electrochemical anodic oxidation is carried out in substrate is that can to adopt common metal be counter electrode, and described common metal is preferably metal platinum; The voltage of described electrochemical anodic oxidation can be 10～25V, and the time of electrochemical anodic oxidation can be 0.5～2h.
2) film of Nano tube array of titanium dioxide that step 1) is obtained is at 0.1～2.5wt%Fe (NO
3)
39H
2Ultrasonic in the solution of O, leave standstill the back and take out drying;
In step 2) in, the described ultransonic time can be 10～40min, and the described time of leaving standstill can be 0～20h.
3) with step 2) described dried composite film thermal treatment, obtain the Nano tube array of titanium dioxide that ferric oxide nanometer particle is modified.
In step 3), described heat treated temperature can be 350～600 ℃, and heat treatment period can be 1.5～2.5h.
The present invention adopts method ultrasonic and that electroless plating combines, and by regulation and control Fe (NO
3)
3The concentration of solution, ultrasonic time and dipping time, controllable deposition ferric oxide nanometer particle in titanium-based titanium dioxide nanotube array surface and pipe, the Nano tube array of titanium dioxide of modifying with ferric oxide nanometer particle can improve TiO on the one hand
2Photocatalysis efficiency; Its photoresponse can be expanded to visible region on the other hand, improve the utilization ratio of sunlight, can improve the receptivity of electrode pair visible light when being applied to photochemical catalysis and the photocatalytic degradation ability of organic pollutant.And preparation process is simple to operate, be easy to realize industrialization.
Description of drawings
The SEM figure of the Nano tube array of titanium dioxide that the ferric oxide that Fig. 1 makes for embodiment 1 is modified.In Fig. 1, scale is 500nm.
The SEM figure of the Nano tube array of titanium dioxide that the ferric oxide that Fig. 2 makes for embodiment 2 is modified.In Fig. 2, scale is 500nm.
The SEM figure of the Nano tube array of titanium dioxide that the ferric oxide that Fig. 3 makes for embodiment 3 is modified.In Fig. 3, scale is 500nm.
The SEM figure of the Nano tube array of titanium dioxide that the ferric oxide that Fig. 4 makes for embodiment 4 is modified.In Fig. 4, scale is 500nm.
The XRD figure of the Nano tube array of titanium dioxide that Fig. 5 modifies for the ferric oxide that makes through 500 ℃ of heat treated pure titinium dioxide nano-tube arrays and embodiment 4.Wherein X-coordinate is diffraction angle 2 θ (degree), and ordinate zou is a diffracted intensity; Curve a is Fe
2O
3-TiO
2, curve b is TiO
2
Embodiment
The invention will be further described below by embodiment.
Embodiment 1
1) base material is the pure titanium plate of thick 2mm, polishes to no marking with abrasive paper for metallograph in the surface, and clean with ultrasonic cleaning in acetone, ethanol and three water, and airing is stand-by.The electrolytic solution of preparation 0.5wt%HF is counter electrode with platinum at room temperature, carries out electrochemical anodic oxidation 30min under 20V voltage, promptly obtains orderly TiO on titanium plate surface
2The nano-tube array rete, nanotube internal diameter 80～90nm, thicknesses of layers is about 500nm.
2) adopt method ultrasonic and that dipping combines, preparation Fe
2O
3Nano-particle modified TiO
2Nano-tube array.Prepared sample in the step (1) is placed 0.1mol/L Fe (NO earlier
3)
3Ultrasonic 40min in the solution takes out and uses distilled water flushing, standing and drying.Sample is calcined 2h under 400 ℃ of conditions, naturally cooling promptly makes Fe then
2O
3Nano-particle modified TiO
2Nano-tube array.As can be seen from Figure 1, small amount of Fe
2O
3Nanoparticle deposition is in TiO
2Between the nanotube mouth of pipe and pipe.The EDS spectrogram shows that this composite membrane is elementary composition by Ti, O and three kinds of Fe, and quantitative analysis shows that the atomic percent of Fe is 0.22%.
3) with Fe
2O
3Nano-particle modified TiO
2Nano-tube array is put into the methylene blue solution of 13.5mg/L as photocatalyst, and through the halogen tungsten lamp irradiation of 500W, test light is according to the concentration of different time methylene blue, according to formula ln (C under magnetic agitation
0/ C
t)=kt is (in the formula: C
0, C
tBe respectively the concentration of initial sum illumination t solution after the time, k is the superfacial velocity constant) the linear fit experimental data, try to achieve apparent speed constant k value, the results are shown in Table 1.The k value is big more, and photocatalytic speed is big more.
Embodiment 2
1) TiO
2The preparation of nano-tube array rete is with embodiment 1.
2) adopt method ultrasonic and that dipping combines, preparation Fe
2O
3Nano-particle modified TiO
2Nano-tube array.Prepared sample in the step (1) is placed 0.5mol/L Fe (NO earlier
3)
3Ultrasonic 8min in the solution takes out and uses distilled water flushing, standing and drying.Sample is calcined 2h under 450 ℃ of conditions, naturally cooling promptly makes Fe then
2O
3Nano-particle modified TiO
2Nano-tube array.As can be seen from Figure 2, Fe
2O
3Nano granule particulate amount obviously increases than Fig. 1, and some nano particles are deposited in the nanotube.The EDS quantitative analysis results shows that the atomic percent of Fe is 0.77%.
3) Fe
2O
3Nano-particle modified TiO
2The test of the apparent speed constant k of nano-tube array photocatalyst visible light photocatalytic degradation methylene blue the results are shown in Table 1 with embodiment 1.
Embodiment 3
1) TiO
2The preparation of nano-tube array rete is with embodiment 1.
2) adopt method ultrasonic and that dipping combines, preparation Fe
2O
3Nano-particle modified TiO
2Nano-tube array.Obtained sample in the step (1) is placed 0.5mol/L Fe (NO earlier
3)
3Ultrasonic 15min in the solution takes out and uses distilled water flushing, standing and drying.Sample is calcined 2h under 500 ℃ of conditions, naturally cooling promptly makes Fe then
2O
3Nano-particle modified TiO
2Nano-tube array.As can be seen from Figure 3, Fe
2O
3The amount of nano particle obviously increases than Fig. 2, and a large amount of nano particles are deposited in the nanotube.The EDS quantitative analysis results shows that the atomic percent of Fe is 1.18%.
3) Fe
2O
3Nano-particle modified TiO
2The test of the apparent speed constant k of nano-tube array photocatalyst visible light photocatalytic degradation methylene blue the results are shown in Table 1 with embodiment 1.
Embodiment 4
1) TiO
2The preparation of nano-tube array rete is with embodiment 1.
2) adopt method ultrasonic and that dipping combines, preparation Fe
2O
3Nano-particle modified TiO
2Nano-tube array.Resultant sample in the step (1) is placed 2.0mol/L Fe (NO earlier
3)
3Ultrasonic 20min in the solution takes out and uses distilled water flushing, standing and drying.Sample is calcined 2h under 550 ℃ of conditions, naturally cooling promptly makes Fe then
2O
3Nano-particle modified TiO
2Nano-tube array.As can be seen from Figure 4, Fe
2O
3The amount of nano particle obviously increases than Fig. 3, some TiO
2Nanotube is covered fully by nano particle.The EDS quantitative analysis results shows that the atomic percent of Fe is 1.58%.Fig. 5 is Fe shown in Figure 4
2O
3Nano-particle modified TiO
2Nano-tube array and through 500 ℃ of heat treated pure TiO
2The XRD figure of nano-tube array.As can be seen from Figure 5, the TiO in two kinds of materials
2Be anatase crystal, Fe
2O
3Nano-particle modified TiO
2Fe has appearred in nano-tube array
2O
3Characteristic peak, confirmed that sedimentary nano particle is Fe
2O
3
3) Fe
2O
3Nano-particle modified TiO
2The test of the apparent speed constant k of nano-tube array photocatalyst visible light photocatalytic degradation methylene blue the results are shown in Table 1 with embodiment 1.
Table 1
Claims (9)
1. the preparation method of the Nano tube array of titanium dioxide modified of ferric oxide nanometer particle is characterized in that may further comprise the steps:
1) with the substrate material surface cleaning pretreatment, prepare electrolytic solution then, electrochemical anodic oxidation is carried out in substrate, can construct one deck at substrate surface and arrange film of Nano tube array of titanium dioxide orderly, controllable size;
2) film of Nano tube array of titanium dioxide that step 1) is obtained is at 0.1～2.5wt%Fe (NO
3)
39H
2Ultrasonic in the solution of O, leave standstill the back and take out drying;
3) with step 2) described dried composite film thermal treatment, obtain the Nano tube array of titanium dioxide that ferric oxide nanometer particle is modified.
2. the preparation method of the Nano tube array of titanium dioxide that ferric oxide nanometer particle as claimed in claim 1 is modified is characterized in that in step 1) described base material is pure titanium material.
3. the preparation method of the Nano tube array of titanium dioxide that ferric oxide nanometer particle as claimed in claim 1 is modified, it is characterized in that in step 1), described cleaning surfaces pre-treatment is to adopt acetone, second alcohol and water that substrate material surface is carried out ultrasonic cleaning successively.
4. the preparation method of the Nano tube array of titanium dioxide that ferric oxide nanometer particle as claimed in claim 1 is modified is characterized in that in step 1) described electrolytic solution is the aqueous solution of 0.1～1.5wt%HF.
5. the preparation method of the Nano tube array of titanium dioxide that ferric oxide nanometer particle as claimed in claim 1 is modified is characterized in that in step 1), and the described condition that electrochemical anodic oxidation is carried out in substrate is that to adopt common metal be counter electrode.
6. the preparation method of the Nano tube array of titanium dioxide that ferric oxide nanometer particle as claimed in claim 5 is modified is characterized in that in step 1) described common metal is a metal platinum.
7. the preparation method of the Nano tube array of titanium dioxide of modifying as claim 1 or 5 described ferric oxide nanometer particles is characterized in that in step 1) the voltage of described electrochemical anodic oxidation is 10～25V, and the time of electrochemical anodic oxidation is 0.5～2h.
8. the preparation method of the Nano tube array of titanium dioxide that ferric oxide nanometer particle as claimed in claim 1 is modified is characterized in that in step 2) in, described ultransonic time 10～40min, the described time of leaving standstill is 0～20h.
9. the preparation method of the Nano tube array of titanium dioxide that ferric oxide nanometer particle as claimed in claim 1 is modified is characterized in that in step 3) described heat treated temperature is 350～600 ℃, and heat treatment period is 1.5～2.5h.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102244275A (en) * | 2011-05-13 | 2011-11-16 | 中国计量学院 | Metal electrode of redox flow battery and preparation method thereof |
| CN102691071A (en) * | 2012-06-01 | 2012-09-26 | 浙江大学 | Preparation method for iron-doped tungsten trioxide photoelectrode |
| CN102718491A (en) * | 2012-03-02 | 2012-10-10 | 海南大学 | Nanotube / powder blending phase metal oxide |
| CN103014810A (en) * | 2011-09-20 | 2013-04-03 | 同济大学 | Ferrotitanium oxide nano-tube array photoanode, preparation method and applications thereof |
| CN104233206A (en) * | 2014-06-30 | 2014-12-24 | 左娟 | Preparation method and application of Fe-doped nanotube array membrane |
| CN106756897A (en) * | 2016-11-15 | 2017-05-31 | 重庆科技学院 | Ag doped ferric oxide nano-tube array structure films and preparation method thereof |
| CN107151039A (en) * | 2016-03-03 | 2017-09-12 | 汉阳大学校产学协力团 | Use the method for treating water of stainless steel nano-tube array |
| CN112058262A (en) * | 2020-09-07 | 2020-12-11 | 西安近代化学研究所 | Iron-titanium composite catalyst, preparation method and application |
| CN112387296A (en) * | 2019-08-16 | 2021-02-23 | 吉林师范大学 | Multi-element co-doped visible-light-driven photocatalyst |
| CN113398904A (en) * | 2021-05-06 | 2021-09-17 | 桂林电子科技大学 | Preparation method and application of catalyst for medium-low temperature photo-thermoelectric synergistic catalytic oxidation of VOCs (volatile organic compounds) |
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2010
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| CN102244275A (en) * | 2011-05-13 | 2011-11-16 | 中国计量学院 | Metal electrode of redox flow battery and preparation method thereof |
| CN103014810B (en) * | 2011-09-20 | 2016-03-30 | 同济大学 | Ferro-titanium oxide nanotube array light anode and preparation and application thereof |
| CN103014810A (en) * | 2011-09-20 | 2013-04-03 | 同济大学 | Ferrotitanium oxide nano-tube array photoanode, preparation method and applications thereof |
| CN102718491A (en) * | 2012-03-02 | 2012-10-10 | 海南大学 | Nanotube / powder blending phase metal oxide |
| CN102691071B (en) * | 2012-06-01 | 2014-11-26 | 浙江大学 | Preparation method for iron-doped tungsten trioxide photoelectrode |
| CN102691071A (en) * | 2012-06-01 | 2012-09-26 | 浙江大学 | Preparation method for iron-doped tungsten trioxide photoelectrode |
| CN104233206A (en) * | 2014-06-30 | 2014-12-24 | 左娟 | Preparation method and application of Fe-doped nanotube array membrane |
| CN104233206B (en) * | 2014-06-30 | 2017-12-19 | 厦门理工学院 | A kind of preparation method and applications of Fe dopen Nanos pipe array films |
| CN107151039A (en) * | 2016-03-03 | 2017-09-12 | 汉阳大学校产学协力团 | Use the method for treating water of stainless steel nano-tube array |
| CN107151039B (en) * | 2016-03-03 | 2021-04-16 | 汉阳大学校产学协力团 | Water treatment method using stainless steel nanotube array |
| CN106756897A (en) * | 2016-11-15 | 2017-05-31 | 重庆科技学院 | Ag doped ferric oxide nano-tube array structure films and preparation method thereof |
| CN112387296A (en) * | 2019-08-16 | 2021-02-23 | 吉林师范大学 | Multi-element co-doped visible-light-driven photocatalyst |
| CN112058262A (en) * | 2020-09-07 | 2020-12-11 | 西安近代化学研究所 | Iron-titanium composite catalyst, preparation method and application |
| CN112058262B (en) * | 2020-09-07 | 2023-02-14 | 西安近代化学研究所 | Iron-titanium composite catalyst, preparation method and application |
| CN113398904A (en) * | 2021-05-06 | 2021-09-17 | 桂林电子科技大学 | Preparation method and application of catalyst for medium-low temperature photo-thermoelectric synergistic catalytic oxidation of VOCs (volatile organic compounds) |
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