CN103866370B - A kind of method of preparing hypoxemia titania nanotube array - Google Patents
A kind of method of preparing hypoxemia titania nanotube array Download PDFInfo
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- CN103866370B CN103866370B CN201210532541.XA CN201210532541A CN103866370B CN 103866370 B CN103866370 B CN 103866370B CN 201210532541 A CN201210532541 A CN 201210532541A CN 103866370 B CN103866370 B CN 103866370B
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Abstract
The present invention relates to a kind of method of preparing hypoxemia titania nanotube array, be included in titanium substrate surface makes Nano tube array of titanium dioxide step 1 by anodic oxidation, with taking described Nano tube array of titanium dioxide as negative electrode, graphite cake is the step 2 that anode is reduced into described Nano tube array of titanium dioxide by electrochemical reduction hypoxemia titania nanotube array. The prepared hypoxemia titanium oxide nanotubes of preparation in accordance with the present invention is black, and optical absorption is good; Targeted electronic that can integrated nanometer pipe transports the low energy gap width advantage of performance and hypoxemia titanium oxide; Widen titanium oxide in field application such as photovoltaic, photocatalysis, fuel cells. Preparation technology of the present invention all carries out in room temperature, and environmental protection is simple to operate, and controllability is strong, is easy to apply.
Description
Technical field
The present invention relates to a kind of method of preparing hypoxemia titania nanotube array on titanium base material surface, be specifically related to oneCan maintain titania nanotube array " tubular structure " constant, at room temperature be changed into the method for hypoxemia titanium oxide. Belong toThe preparation of photocatalysis/photovoltaic device material and field of nanometer technology.
Background technology
Early 1970s, global energy crisis impels people more and more pay attention to the exploitation of solar utilization technique and answerWith. Fujishima etc. [Nature1972,37,238-245] report titanium dioxide (TiO in 19722) in the time of light irradiation sustainablyBe hydrogen by water decomposition. Cause the photocatalysis oxidation technique of titanium dioxide to be developed rapidly. Titanium dioxide by photoactivation be due toIt absorbs after light energy (hv), and the electronics in valence band will be excited to conduction band, forms electronegative high activity electronics e-, withTime in valence band, produce the hole h of positively charged+, form redox system (reaction equation 1), and activating reaction formula 2-4, enter oneStep generates the group (as hydroxyl, OH) of high reaction activity, being adsorbed on TiO2The organic pollutant degradation on surface is CO2、H2O, is oxidized or is reduced to harmless object [ChemRev1995,95,69-96.] inorganic pollution;
TiO2+hv→h++e-(1)
h++H2O→OH·+H+,(2)
h++OH-→OH·,(3)
2e-+2H+→H2,(4)
In recent years, because the electron transport performance of titania nanotube is better than granular materials, in photovoltaic, photocatalysis, sensingThere is important application prospect in field, enjoy academia to pay close attention to [Angew.Chem.Int.Ed.2011,50,2904-2939]. Scientific researchWorkers pass through TiO2Doping, modification and the nanostructured of nanotube are constructed, and have improved to some extent its photocatalysis and have livedProperty and photoelectric transformation efficiency [Chem.Rev.2007,107,2891-2959]. But reaction equation 1 is with good conditionsi: only haveEnergy (hv) is greater than titanium dioxide energy gap (Eg) photon while injecting, formula 1 just can be carried out to the right. Because titanium dioxide is wideBandgap semiconductor (Eg≈ 3eV), therefore only have effectively activating reaction formula 1 of ultraviolet light, this has just limited titanium dioxide at the sunCan utilize the application (visible ray can not activate titanium dioxide) of aspect. For this reason, people adopt various doping methods to titanium oxide modification[Science2011,331,746-50; Science2001,293,269-71], reduce the broadband, forbidden band of titanium dioxide certain journeyDegree has been expanded the photoactivation performance of titanium oxide at visible region. Compared with titanium dioxide, hypoxemia titanium oxide due to its energy gapNarrow easy absorption visible ray and obtain the fields such as photovoltaic, photocatalysis, fuel cell extensive concern [Chem.Commun., 2012,48,7949-7951]. But the method that present stage is prepared hypoxemia titanium oxide is mainly heat more than 1000 DEG C with hydrogen or titanium valveReduction titanium dioxide [Science2011,331,746-750]. Under such hot conditions, prepare nanoscale hypoxemia titanium oxide ratioMore difficult. Use strong reductant CaH2To titanium dioxide long time treatment (350 DEG C, 15 days), also can only obtain hypoxemia oxygenChange titanium nano particle [Angew.Chem.Int.Ed.2011,50,7418-7421].
From above-mentioned, the low energy gap width advantage that the targeted electronic of nanotube is transported to performance and hypoxemia titanium oxide is integrated,To greatly widen titanium oxide in field application such as photovoltaic, photocatalysis, fuel cells.
Summary of the invention
Ordering pransition rule based on oxygen room in thin film of titanium oxide under electric field action, for titanium dioxide energy gapWider (Eg≈ 3eV), can not absorb the problem of visible ray, the object of the present invention is to provide one to prepare hypoxemia titanium oxide nanotubesThe method of array, integrated the targeted electronic of nanotube is transported to the low energy gap width advantage of performance and hypoxemia titanium oxide, thus carryThe absorbing properties of high oxidation titanium, greatly widens titanium oxide in field application such as photovoltaic, photocatalysis, fuel cells.
The method of preparing hypoxemia titania nanotube array of the present invention, comprising: at titanium substrate surface by anodic oxidation systemObtain the step 1 of Nano tube array of titanium dioxide, and taking described Nano tube array of titanium dioxide as negative electrode, graphite cake is that anode passes throughElectrochemical reduction is reduced into described Nano tube array of titanium dioxide the step 2 of hypoxemia titania nanotube array.
Described step 1 and step 2 are all at room temperature carried out, and therefore can not change titanium oxide nanotube array structure.
Preferably, the electrolyte that described anodic oxidation adopts is the second containing 0.1～1.0wt% ammonium fluoride and 1～10vol% waterGlycol solution.
Again, described anodised anodic oxidation voltage can be 30～80V, and oxidization time can be 1～12h.
The extra electric field of described electrochemical reduction can be provided by dc source. Voltage is given according to cathodic surface area sizeFixed, be 1～10V/cm2, and keep 0.5h～12h.
Again, the electrolyte of described electrochemical reduction can be conductivity water solution. Its electrolyte is the thing that can make water conduction after dissolvingMatter, is preferably NaOH. The addition of NaOH can be 1～10g/L.
In the present invention, described titanium base material can be pure titanium or titanium alloy.
The prepared hypoxemia titanium oxide nanotubes of preparation in accordance with the present invention is black, and optical absorption is good; Can be integratedThe targeted electronic of nanotube transports the low energy gap width advantage of performance and hypoxemia titanium oxide; Widen titanium oxide photovoltaic, photocatalysis,The field application such as fuel cell.
Preparation technology of the present invention all carries out in room temperature, and environmental protection is simple to operate, and controllability is strong, is easy to apply.
Brief description of the drawings
Fig. 1 is the digital camera photo of titania nanotube array before and after embodiment 1 electrochemical reduction;
Fig. 2 is ESEM (SEM) photo of titania nanotube array before and after embodiment 1 electrochemical reduction;
Fig. 3 is the ultraviolet-visible spectrophotometer test result of titania nanotube array before and after embodiment 1 electrochemical reduction;
Fig. 4 is the digital camera photo of titania nanotube array before and after embodiment 2 electrochemical reductions;
Fig. 5 is ESEM (SEM) photo of hypoxemia titania nanotube array after embodiment 2 electrochemical reductions;
Fig. 6 is ESEM (SEM) photo of hypoxemia titania nanotube array after embodiment 2 electrochemical reductions;
Fig. 7 is x-ray photoelectron spectroscopy (XPS) the titanium 2p High Resolution Spectrum seam of titania nanotube array before and after embodiment 2 electrochemical reductionsGap;
Fig. 8 is the digital camera photo of titania nanotube array before and after embodiment 3 electrochemical reductions;
Fig. 9 is the ultraviolet-visible spectrophotometer test result of hypoxemia titania nanotube array after embodiment 3 electrochemical reductions;
Figure 10 is the digital camera photo of titania nanotube array before and after embodiment 4 electrochemical reductions;
Figure 11 is surface topography ESEM (SEM) photo of the prepared hypoxemia titania nanotube array of embodiment 4;
Figure 12 is the ultraviolet-visible spectrophotometer test result of titania nanotube array before and after embodiment 4 electrochemical reductions.
Detailed description of the invention
Further illustrate the present invention below in conjunction with accompanying drawing and following embodiment, should be understood that following embodiment and/or accompanying drawingOnly for the present invention is described, and unrestricted the present invention.
The method of preparing hypoxemia titania nanotube array of the present invention, comprising: at titanium substrate surface by anodic oxidation systemObtain the step 1 of Nano tube array of titanium dioxide, and taking described Nano tube array of titanium dioxide as negative electrode, graphite cake is that anode passes throughElectrochemical reduction is reduced into described Nano tube array of titanium dioxide the step 2 of hypoxemia titania nanotube array.
More specifically, as example, the present invention can comprise the following steps:
A) adopt anodizing technology to prepare Nano tube array of titanium dioxide, anodic oxygen on base material (can be pure titanium or titanium alloy) surfaceChange electrolyte is ethylene glycol solution, containing 0.1～1.0wt% ammonium fluoride and 1～10vol% water; Anodic oxidation voltage is 30～80V, oxidization time is 1h～12h;
B) adopt electrochemical techniques at room temperature Nano tube array of titanium dioxide to be reduced into the hypoxemia titania nanotube array of black.
Step b) in, electrochemical reduction can carry out in conductivity water solution, taking nano-tube array as negative electrode, graphite cakeFor anode, extra electric field, and keep certain hour.
Wherein, electrochemical reduction conductivity water solution can be NaOH solution, the addition of electrolyte NaOH is 1～10g/L。
Again, extra electric field can be provided by dc source, and voltage is given with reference to cathodic surface area size, is 1～10V/cm2；The retention time of extra electric field is 0.5h～12h.
The present invention has the following advantages:
1, electrochemical reduction technology of the present invention is at room temperature carried out;
2, electrochemical reduction technology of the present invention can not change titanium oxide nanotube array structure;
3, the prepared hypoxemia titania nanotube array of electrochemical reduction technology of the present invention, optical absorption is good;
4, the targeted electronic transport property that the prepared hypoxemia titania nanotube array of electrochemical reduction technology of the present invention can integrated nanometer pipeCan with the low energy gap width advantage of hypoxemia titanium oxide;
5, the prepared hypoxemia titania nanotube array of electrochemical reduction technology of the present invention can widen titanium oxide photovoltaic, photocatalysis,The field application such as fuel cell;
6, preparation technology of the present invention is simple to operate, and controllability is strong, is easy to apply.
Further exemplify embodiment below to describe the present invention in detail. Should be understood that equally following examples are only for to thisBright being further described, can not be interpreted as limiting the scope of the invention, and those skilled in the art is according to of the present inventionSome nonessential improvement that foregoing is made and adjustment all belong to protection scope of the present invention. Temperature that following example is concrete,, those skilled in the art can be by explanation herein time, technological parameter etc. are only also examples in OK range,Do in suitable scope and select, and do not really want to be defined in the below concrete numerical value of example.
Embodiment 1
(a) first adopt anodizing technology to prepare Nano tube array of titanium dioxide on pure titanium surface, anodic oxidation electrolyte is that ethylene glycol is moltenLiquid, containing 0.1wt% ammonium fluoride and 10vol% water; Anodic oxidation voltage is 80V, and oxidization time is 1h; (b) after again in room temperatureNano-tube array is carried out to electrochemical reduction processing, and electrochemical reduction carries out in NaOH solution, taking nano-tube array as cloudyThe utmost point, graphite cake is anode, applying voltage is 10V/cm2, the addition of NaOH is 1g/L, the processing time is 12h;
Khaki (titania nanotube) when electrochemical reduction is processed rear nano-tube array from anodic oxidation becomes black (Fig. 1),Formed by hypoxemia titanium oxide according to analyzing this black oxidation titanium nanotube. Fig. 2 is titanium oxide before and after the present embodiment electrochemical reductionESEM (SEM) photo of nano-tube array, processes and can not change nano-tube array surface shape from the known electrochemical reduction of this figureLooks. Fig. 3 is the ultraviolet-visible spectrophotometer test knot of titania nanotube array before and after the present embodiment electrochemical reductionReally, wherein curve 1,2,3 represents respectively after Nano tube array of titanium dioxide after pure titanium, anodic oxidation, electrochemical reductionHypoxemia titania nanotube array, this result shows that the photo absorption performance of the rear nano-tube array of electrochemical reduction processing has significantly raising.
Embodiment 2
(a) first adopt anodizing technology to prepare Nano tube array of titanium dioxide on pure titanium surface, anodic oxidation electrolyte is that ethylene glycol is moltenLiquid, containing 0.6wt% ammonium fluoride and 8vol% water; Anodic oxidation voltage is 30V, and oxidization time is 12h; (b) after again in room temperatureNano-tube array is carried out to electrochemical reduction processing, and electrochemical reduction carries out in NaOH solution, taking nano-tube array as cloudyThe utmost point, graphite cake is anode, applying voltage is 1V/cm2, the addition of NaOH is 10g/L, the processing time is 0.5h;
Light yellow (titania nanotube) (left figure of Fig. 4) when electrochemical reduction is processed rear nano-tube array by anodic oxidation becomes blackLook (the right figure of Fig. 4). Referring to Fig. 7, it illustrates the X-ray electronic energy of the present embodiment electrochemical reduction front and back titania nanotube arraySpectrum (XPS) titanium 2p High Resolution Spectrum gap, wherein curve 1,2 represent respectively Nano tube array of titanium dioxide after anodic oxidation,Nano-tube array after electrochemical reduction, this result shows the rear product surface Ti of electrochemical reduction processing3+Peak is more remarkable, shows placeAfter reason, product is hypoxemia phase. Fig. 5 is the ESEM (SEM) of hypoxemia titania nanotube array after the present embodiment electrochemical reductionPhoto, processes and can not change nano-tube array surface topography from the known electrochemical reduction of this figure. Its cross section stereoscan photograph is shown inFig. 6, after visible processing, nanotube pattern can keep.
Embodiment 3
(a) first adopt anodizing technology to prepare Nano tube array of titanium dioxide on pure titanium surface, anodic oxidation electrolyte is that ethylene glycol is moltenLiquid, containing 0.1wt% ammonium fluoride and 10vol% water; Anodic oxidation voltage is 50V, and oxidization time is 2h; (b) after again in room temperatureNano-tube array is carried out to electrochemical reduction processing, and electrochemical reduction carries out in NaOH solution, taking nano-tube array as cloudyThe utmost point, graphite cake is anode, applying voltage is 6V/cm2, the addition of NaOH is 5g/L, the processing time is 3h;
Yellow (titania nanotube) (the left figure of Fig. 8) when electrochemical reduction is processed rear nano-tube array from anodic oxidation becomes black(the right figure of Fig. 8), is made up of hypoxemia titanium oxide according to analyzing this black oxidation titanium nanotube. Fig. 9 illustrates the present embodiment electrochemistryAfter reduction, the ultraviolet-visible spectrophotometer test result of hypoxemia titania nanotube array, in contrast to the curve 2 in Fig. 3,The photo absorption performance that can find out the rear nano-tube array of electrochemical reduction processing has significantly raising.
Embodiment 4
(a) first adopt anodizing technology to prepare Nano tube array of titanium dioxide on pure titanium surface, anodic oxidation electrolyte is that ethylene glycol is moltenLiquid, containing 0.1wt% ammonium fluoride and 10vol% water; Anodic oxidation voltage is 50V, and oxidization time is 2h; (b) after again in room temperatureNano-tube array is carried out to electrochemical reduction processing, and electrochemical reduction carries out in NaOH solution, taking nano-tube array as cloudyThe utmost point, graphite cake is anode, applying voltage is 2V/cm2, the addition of NaOH is 8g/L, the processing time is 6h;
Light yellow (titania nanotube) (left figure of Figure 10) when electrochemical reduction is processed rear nano-tube array by anodic oxidation becomesBlack (the right figure of Figure 10), is made up of hypoxemia titanium oxide according to analyzing this black oxidation titanium nanotube. Figure 11 is the present embodiment instituteSurface topography ESEM (SEM) photo of the hypoxemia titania nanotube array of preparation, from the known electrochemical reduction processing of this figureCan not change nano-tube array surface topography. Figure 12 be titania nanotube array before and after the present embodiment electrochemical reduction ultraviolet-Visible spectrophotometer test result, the nano titania that wherein curve 1,2,3 represents respectively after pure titanium, anodic oxidationHypoxemia titania nanotube array after pipe array, electrochemical reduction, this result shows the rear nano-tube array of electrochemical reduction processingLight reflectivity significantly reduce, display light absorbent properties improve significantly.
Industrial applicability: the hypoxemia titania nanotube array prepared according to the present invention has nanostructured extinction and materialIntrinsic extinction feature, light absorpting ability is strong. The method of preparing hypoxemia titania nanotube array of the present invention is all carried out in room temperature,Environmental protection, simple for process, can be used for the preparation of catalysis material and electrooptical device electrode material, at photovoltaic, lightThe field such as catalysis, fuel cell has practical value.
Claims (9)
1. prepare the method for hypoxemia titania nanotube array for one kind, it is characterized in that, be included in titanium substrate surface makes Nano tube array of titanium dioxide step 1 by anodic oxidation, with taking described Nano tube array of titanium dioxide as negative electrode, graphite cake is the step 2 that anode is reduced into described Nano tube array of titanium dioxide by electrochemical reduction hypoxemia titania nanotube array, and the extra electric field of described electrochemical reduction is 1～10V/cm2, keeping 0.5h～12h, described step 2 is at room temperature carried out.
2. the method for preparing hypoxemia titania nanotube array according to claim 1, is characterized in that, described step 1 and step 2 are all at room temperature carried out.
3. the method for preparing hypoxemia titania nanotube array according to claim 1, is characterized in that, the electrolyte that described anodic oxidation adopts is the ethylene glycol solution containing 0.1～1.0wt% ammonium fluoride and 1～10vol% water.
4. the method for preparing hypoxemia titania nanotube array according to claim 1, is characterized in that, described anodised anodic oxidation voltage is 30～80V, and oxidization time is 1～12h.
5. the method for preparing hypoxemia titania nanotube array according to claim 1, is characterized in that, described extra electric field is provided by dc source.
6. the method for preparing hypoxemia titania nanotube array according to claim 5, is characterized in that, the electrolyte in the electrolyte that described electrochemical reduction adopts is the material that can make water conduction after dissolving.
7. the method for preparing hypoxemia titania nanotube array according to claim 6, is characterized in that, described electrolyte is NaOH.
8. the method for preparing hypoxemia titania nanotube array according to claim 7, is characterized in that, the addition of NaOH is 1～10g/L.
9. according to the method for preparing hypoxemia titania nanotube array described in any one in claim 1 to 8, it is characterized in that, described titanium base material is pure titanium or titanium alloy.
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