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Photo-catalytic degradation of Rhodamine B on C-, S-, N-, and Fe-doped TiO2

Photo-catalytic degradation of Rhodamine B on C-,S-,N-,and Fe-doped TiO2 under visible-light irradiation

Xiangxin Yang a,1,Chundi Cao a,Larry Erickson a,Keith Hohn a,Ronaldo Maghirang b,Kenneth Klabunde c,*

a Department of Chemical Engineering,Kansas State University,Manhattan,KS66506,USA

b Department of Biological and Agricultural Engineering,Kansas State University,Manhattan,KS66506,USA

c Department of Chemistry,Kansas State University,Manhattan,KS66506,USA

1.Introduction

Titanium dioxide(TiO2),as a chemically stable,nontoxic,highly ef?cient,and relatively inexpensive photocatalyst,has been widely used for water and air puri?cation since many environmental pollutants can be degraded by oxidation and reduction processes on TiO2surface.[1–3]Under irradiation with light of suf?cient energy to span TiO2’s band gap,the electron(eà)can be promoted into the conduction band(CB),leaving a hole(h+)in the valence band(VB).Then,electrons and holes can initiate redox reactions on the surface of TiO2.Finally,pollutants can be degraded into CO2and H2O[1].However,the application of TiO2is limited by its UV activation requirement because of its large band gap(3.2or3.0eV in the anatase or rutile crystalline phase,respectively).Therefore, efforts have been directed towards shifting the optical sensitivity of TiO2from UV to the visible-light region for the ef?cient use of solar energy,which is composed of only about2–3%UV light.[4] Transition metal dopants have been widely used to extend TiO2’s light absorption into the visible-light region.Iron is frequently employed owing to its unique half-?lled electronic con?guration,which might narrow the energy gap through the formation of new intermediate energy levels.[5]Choi et al.[6] studied the effects of21different dopants on the photoreactivity of TiO2.Fe3+dopant proved to be better than Ru3+,V4+,Mo5+,Os3+, and Re5+.At0.1–0.5wt.%,the photocatalytic activity for the reduction of CCl4and the oxidation of CHCl3was signi?cantly increased.Fe-doped TiO2also exhibited enhanced activity under visible-light irradiation for the degradation of methylene blue (MB),[5]methylene orange(MO),[7]methanol,[8]toluene,[9] and disinfection of E.Coli suspension.[10]It is generally accepted that the Fe3+dopant formed shallow charge traps within the TiO2 crystal lattice through the substitution of Ti4+,which reduced the electron–hole recombination and improved the photocatalytic ef?ciency[8,11,12].

Although transition metal modi?ed TiO2photocatalysts are active under visible-light irradiation,the ef?ciency is still low for practical use.Recently,doping nonmetal atoms,such as C,N,and S, has received much attention.Theoretical calculations showed that the p-orbitals of these dopants signi?cantly overlapped with the valence band O2p-orbitals,which facilitated the transport of photo-generated charge carriers to the surface of the catalyst. Wang et al.[13]reported the shift of photo response of TiO2from UV to the infrared region by a carbon dopant.S-doped TiO2showed

Applied Catalysis B:Environmental91(2009)657–662

A R T I C L E I N F O

Article history:

Received4April2009

Received in revised form8June2009 Accepted9July2009

Available online17July2009

Keywords:

Carbon

Nitrogen

Sulfur

Iron

Dopants

TiO2

Photocatalyst A B S T R A C T

C-,S-,N-,and Fe-doped TiO2photocatalysts were synthesized by a facile sol–gel method.The structure and properties of catalysts were characterized by N2desorption–adsorption,X-ray diffraction(XRD), UV–vis spectroscopy,and X-ray photoelectron spectroscopy(XPS).Results revealed that the surface area of the multi-doped TiO2was signi?cantly increased and the crystallite size was smaller than the pure TiO2obtained by a similar https://www.wendangku.net/doc/9b7878318.html,pared with TiO2,the peak position in doped-TiO2XRD patterns was slightly shifted,which could be attributed to the distortion by the substitution of carbon,nitrogen,and sulfur dopants for some oxygen atoms and Fe3+for Ti4+in the lattice of TiO2.These substitutions were con?rmed by XPS.In addition,these dopants were responsible for narrowing the band gap of TiO2and shifting its optical response from ultraviolet(UV)to the visible-light region.The photocatalytic reactivities of these multi-doped TiO2catalysts were investigated by degrading Rhodamine B(RB)in aqueous solution under visible-light irradiation(l>420nm).It was found out that the reactivity was signi?cantly enhanced and the catalyst doped with nitrogen,carbon,sulfur,and0.3wt%iron had the highest photocatalytic activity.

*Corresponding author.Fax:+17855326666.

E-mail address:kenjk@https://www.wendangku.net/doc/9b7878318.html,(K.Klabunde).

1Current email address:tonyjone568@https://www.wendangku.net/doc/9b7878318.html,.Contents lists available at ScienceDirect

Applied Catalysis B:Environmental

j o u rn a l h om e p a ge:w w w.e l s e v i e r.c o m/l o c a t e/a p ca t b

doi:10.1016/j.apcatb.2009.07.006

high activity for degradation of MB in water under irradiation at wavelengths longer than440nm.[14]Visible-light-active N-doped TiO2photocatalyst has been prepared by thermal nitridation of TiO2,amination of TiO2,sputtering,and hydrolyzing titanium-precursors in ammonia.[15–18]

It is of great interest to investigate the synergetic effects of multiple dopants on the optical shift,crystallinity,surface areas, and activity of TiO2.It was reported that N and F co-doped TiO2had higher visible-light activity than N-doped or F-doped TiO2since N dopant improved the visible-light absorption and the doped F atom enhanced the surface acidity and the adsorption of agents.[19] Tryba[20]synthesized C and Fe co-doped TiO2and it showed higher activity than TiO2for the decomposition of phenol in multiple uses.Our previous research showed two dopants had more bene?cial effects than a single one for enhancing the absorption in the visible-light region and improving the photo-catalytic activity of TiO2.[21,22]In this work,multiple dopants-modi?ed TiO2,namely,C,N,S,and Fe,were developed via a facile sol–gel process,which showed an enhanced activity compared to TiO2owing to the modi?cation by these dopants.

2.Experimental

2.1.Catalyst synthesis

Thiourea was used as the precursor for nonmetal atoms and iron chloride as the iron precursor.These two compounds and titanium isopropoxide(97%)were purchased from Aldrich and used without further treatment.The general procedure for the preparation was as follows:First,3.8g thiourea was added to a beaker containing150mL deionized water,which was kept in a water–ice bath.While under vigorous stirring,a certain amount of iron chloride,according to the desired Fe3+doping content,was added to the solution.Next,11mL of titanium isopropoxide was added dropwise to the aqueous solution.The mixture was stirred for12h and aged for24h.Water was removed by drying in air at 808C.The dried powder was ground and calcined at5008C in air for2h.Fe doping content(x)was chosen as0,0.1,0.3,and0.5wt%, which was the mass percentage of Fe3+in the titanium oxide powder(denoted as CNS–x Fe–TiO2).The same procedure,without thiourea and iron chloride,was used to prepare pure TiO2. Commercial Degussa P25TiO2(anatase/rutile=75/25)with a speci?c surface area of50m2/g was used for comparison purposes.

2.2.Catalyst characterization

N2adsorption–desorption isotherms were obtained at77K on a NOVA1000series instrument(Quantachrome,USA).The speci?c surface area was determined by multipoint Brunaer–Emmett–Teller(BET)method using the adsorption data in the relative pressure(P/P0)range of0.05–0.3.Desorption isotherms were used to determine the pore size distribution,pore volume,and pore diameter using the Barret–Joyner–Halender(BJH)method.Prior to measurements,the catalysts were degassed at1508C for1h.

X-ray diffraction(XRD)patterns were obtained with a Bruker D8diffractometer with Cu K a radiation(1.5406)at40kV and 40mA.Measurements were recorded in steps of0.0258with a count time of2s in the2u range of20–658.The phases were identi?ed with the aid of Joint Committee on Powder Diffraction Standards(JCPDS)?les.

UV–vis absorbance spectra of catalysts were recorded with a Cary500Scan UV–vis-NIR spectrophotometer.All spectra were referenced to poly(tetra?uoroethylene).

X-ray photoelectron spectroscopy(XPS)data were recorded using a PerkinElmer PHI5400electron spectrometer.The spectro-meter utilizes achromatic Al K a radiation(1486.6eV).Before samples were tested,the spectrometer was calibrated by setting the binding energies of Au4f7/2and Cu2p3/2to84.0and932.7eV, respectively.Binding energies for the samples were normalized with respect to the position of the C1s peak resulting from adsorbed hydrocarbon fragment.The XPS binding energies were measured with a precision of0.1eV.

2.3.Photocatalytic activity measurements

The photocatalytic activity of catalysts was evaluated by the degradation of Rhodamine B(RB)in an aqueous solution.The light source was a1000W high-pressure Hg arc lamp(Oriel Corpora-tion).The combination of a vis-NIR long pass?lter(400nm)and colored glass?lter(>420nm)was used to eliminate UV radiation during visible-light experiments.A general procedure was carried out as follows:First,100mL aqueous RB solution(1?10à5mol/L) was placed in a water-jacketed reactor,which was maintained at a temperature of258C.Then,30mg catalyst was suspended in the solution.The suspension was stirred vigorously for60min in the dark to establish adsorption–desorption equilibrium of RB.The suspension was then irradiated under visible-light.Samples were withdrawn periodically from the reactor,then centrifuged and analysed by recording variations in the absorption in the UV–vis spectra of RB using a Cary500UV–vis spectrophotometer at its characteristic wavelength(l=553nm).[23–25]The reproduci-bility of the results was checked by repeating the results at least three times and was found to be within acceptable limits(?1%).

3.Results and discussion

3.1.N2adsorption–desorption

Fig.1illustrates N2adsorption–desorption isotherms and pore size distribution of CNS-x Fe-TiO2catalysts.All samples showed isotherms of type IV with an H2hysteresis loop,indicating the mesoporous nature,attributed to the aggregation of TiO2crystal-lites.[26]The BJH analysis yielded a peak at a pore diameter of 5.2nm for TiO2and5.7nm for CNS-x Fe-TiO2,suggesting a very narrow distribution of the mesopore dimensions.Table1sum-marizes the surface area,pore volume,and pore diameter of the catalysts.The CNS-0Fe-TiO2exhibited much higher surface area, pore volume,and pore diameter than pure TiO2.Apparently,these nonmetal atom dopants prevented the aggregation of smaller crystallites,forming larger pores and increasing surface areas. Another remarkable phenomenon was that the addition of an iron dopant further increased the surface area slightly.The bene?cial effect of the iron dopant was attributed to the enhanced lattice strain because of the iron incorporation into the TiO2network and then decreased grain growth rate,i.e.,sintering[5,27].The incorporation of these dopants was further con?rmed by later XRD analysis.

3.2.UV–vis spectroscopy

Fig.2shows UV–vis diffuse re?ectance spectra of the pure and doped-TiO2.As expected,pure TiO2showed absorption only in the UV region(less than400nm),due to the intrinsic band gap absorption of TiO2.The onset of the absorption spectrum of CNS-x Fe-TiO2was shifted towards visible-light,a result of carbon, nitrogen,sulfur,and iron dopants.It has been reported that when O atom of the TiO2lattice was substituted by C,N,or S,the p-orbital of these dopants overlapped with the valence band O2p-orbitals. [17,28].Therefore,the band gap of TiO2became narrower and the absorption edge shifted to the lower energy.In addition,elemental carbon or carbonaceous species could act as photosensitizer and effectively extend the absorption to visible-light region[21,22,29].

X.Yang et al./Applied Catalysis B:Environmental91(2009)657–662 658

With the addition of Fe 3+,the absorbance in the visible-light range was enhanced,which can be attributed to the interaction between Fe 3+d electrons and the TiO 2conduction or valence band since the Fe dopant could introduce impurity levels within the band gap of TiO 2.[30]The electronic transitions between the impurity level and the valence or conduction band effectively red shifted the band edge absorption threshold.[31]The absorption edge shift from UV to the visible-light region apparently indicates there is smaller band gap energy for CNS-x Fe-TiO 2catalysts.3.3.X-ray diffraction

Fig.3exhibits the XRD patterns of pure and doped-TiO 2.The characteristic (101)plane diffraction peak (2u =25.38)of anatase phase is clearly observed.No peaks for the other TiO 2phases (rutile or brookite)appear.For CNS-0Fe-TiO 2,the width of this peak broadened and its intensity was signi?cantly decreased.With the addition of iron,this phenomenon was further enhanced.The average crystallite size was estimated by

the Scherrer equation (d =0.94l /b cos u ,where l was the X-ray wavelength,b was the full width at half maximum of the (101)peak,and u was the half angle of the diffraction peak on the 2u scale).The calculated crystallite size was listed in Table 1.It was obvious that the crystal growth was signi?cantly suppressed by these dopants,consistent with N 2desorption–adsorption results.The effect of nonmetal dopants was more remarkable than that of the iron dopant.With the introduction of iron,the further decrease in crystallite size can be ascribed to the retarding effect of Fe 3+on TiO 2anatase crystallite growth,which favored the formation of smaller TiO 2crystallites [27].We also noticed that for the (101)plane peak,a small shift occurred in the peak position after the introduction of C,N,and S.Therefore,the crystal lattice was distorted by these dopants.Since the radii of

Fe 3+and Ti 4+for coordination number of 6were 0.79and 0.75A

?,respectively,the substitution of Ti 4+site by Fe 3+

ion should be facile without a signi?cant crystalline distortion [6,32].The replacement of Ti 4+by Fe 3+was proven by the further slight shift of the (101)peak with iron introduction.Although the Fe ion content in our samples was increased up to 0.5wt%,no other crystalline phase (Fe 2O 3or Fe x TiO y )could be found.We assumed that iron ions were incorporated into the TiO 2network (replacing Ti 4+or locating at interstitial sites)or well dispersed on the

surface.

Fig.1.N2adsorption–desorption isotherms (A)and pore size distribution (B)of pure TiO 2and CNS-x Fe-TiO 2catalysts.

Table 1

Textural property of catalysts.Catalyst

Surface area (m 2/g)Pore volume (cm 3/g)Pore diameter (nm)Crystallite size (nm)TiO 2

570.14 4.214.0CNS-0Fe-TiO 2960.21 5.749.3CNS-0.1Fe-TiO 2980.22 5.758.9CNS-0.3Fe-TiO 21000.22 5.728.9CNS-0.5Fe-TiO 2

103

0.23

5.71

9.0

Fig.2.The UV diffuse re?ectance spectra of pure TiO 2and CNS-x Fe-TiO 2

catalysts.

Fig.3.XRD patterns of pure TiO2and CNS-x Fe-TiO2catalysts.

X.Yang et al./Applied Catalysis B:Environmental 91(2009)657–662659

3.4.X-ray photoelectron spectroscopy

To investigate the chemical states of dopants in TiO 2,C 1s,N 1s,S 2p,and Fe 2p core levels were measured by XPS.C 1s,N 1s,and S 2p XPS spectra of CNS-0Fe-TiO 2and Fe 2p of CNS-0.3Fe-TiO 2are shown in Fig.4.

The C 1s XPS spectra showed a strong peak at 285eV and a shoulder at around 288eV.After sputtering,a new peak appeared at 281eV.Three forms of carbon species have been previously detected:elemental carbon with binding energy of 285eV;surface-adsorbed carbonate species (288V);Ti–C bond resulting from substituting the lattice oxygen atoms by carbon (281eV)[13,33].Therefore,multiple carbon species,namely,substitutional and interstitial carbon atoms and carbonate species,existed in the lattice of TiO 2.

The S 2p XPS spectrum showed a peak at 168eV.The assignment of this peak was controversial.A broad peak attributed to S 2p 3/2at around 168eV suggested several oxidation states of S atoms:the peak of the S 6+state appeared at 168.2eV and the peak at 167.5eV was assigned to S 4+.[34]However,it was also reported that when SO 2molecules were adsorbed on a TiO 2surface,the peak of the S 2p state was in the region of 166–170eV.[35]The controversy was likely due to different preparation methods or post treatments.It was more reasonable to attribute this peak to S 6+state in our case since we treated the sample in air at 500?C for 2h.After sputtering,a new peak appeared at 160.2eV,indicating that sulfur entered the lattice of TiO 2and substituted for oxygen atoms.

The N 1s XPS spectrum showed a very broad peak between 398and 402eV.Peaks in this region were assigned to chemisorbed N 2molecules and/or N-containing compounds,such as NO x or NH 3formed during the decomposition and oxidation of the N-precursors.[36,37]After sputtering,the broad peak disappeared and a new one was observed at around 396eV,which usually has been assigned to N 2àanions resulting from substitution for oxygen sites by nitrogen atoms in the TiO 2lattice.[38]

The Fe 2P XPS spectrum showed a peak at 709.1eV.The peak can be assigned to Fe 3+.[39,40]The spectra pre and after sputtering were nearly identical,indicating Fe 3+existed both on the surface and inside the bulk of TiO 2powder.

Based on XPS survey spectra after sputtering of CNS-0Fe-TiO 2and CNS-x Fe-TiO 2(not shown here),the atomic concentration of C,N,and S were 6.3,0.2,and 1.8%,respectively.The further addition of iron dopant did not obviously affect the concentration of sulfur and nitrogen,while the carbon content decreased some.At this point,we have not further studied this phenomenon.3.5.Degradation of RB

Characterization results indicate that the optical response of TiO 2was shifted from UV to visible-light region with the introduction of carbon,nitrogen,sulfur,and iron dopants.This implied that these multi-doped TiO 2catalysts,unlike pure TiO 2,might be very active under visible-light irradiation.The investiga-tion of visible-light-activity was carried out by the degradation of RB in an aqueous solution.For the comparison of reaction rate among different catalysts,pseudo-?rst-order reaction equation was introduced as follows:àdC

?kC (1)

where C is the RB concentration at time t and k is the apparent reaction rate constant.This equation can be integrated to give the following form:

àln C 0

?kt (2)

This kinetic model has been successfully applied to various heterogeneous photocatalytic liquid–solid systems,such as Fe(III)-doped TiO 2/methyl orange [41]and anion-doped TiO 2/methylene blue.[42]According to Beer’s law,the absorbance

Fig.4.XPS spectra for the C 1s,N 1s,S 2p core levels of CNS-0Fe-TiO2and Fe 2p of CNS-0.3Fe-TiO2(a:before sputtering;b:after sputtering).

X.Yang et al./Applied Catalysis B:Environmental 91(2009)657–662

660

553nm(the characteristic absorption wavelength of RB)was proportional to the concentration of RB in the reaction solution,so ln(C/C0)equaled ln(A/A0),where A0was the solution absorbance at time zero and A was the solution absorbance at a time t after turning on the lamp.It should be pointed out that the concentration of RB in the aqueous solution decreased before lighting because of adsorp-tion in the dark:the values were6.8,7.5,9.4,9.4,9.6,and9.8%of original RB concentration for P25,TiO2and CNS-x Fe-TiO2with x equals0,0.1,0.3,and0.5,respectively.Most of the concentration decrease occurred during irradiation,therefore,the decrease in RB concentration during irradiation was due to chemical reaction rather than adsorption.For convenience,we assumed that the concentration of RB after desorption–adsorption equilibrium was the initial concentration,C0.Fig.5shows the degradation of RB as a function of reaction time in the presence of different catalysts under visible-light irradiation.According to the above kinetic model,the rate constants k were found to be0.0010,0.0016,0.0029,and 0.0019minà1for CNS-x Fe-TiO2with x equals0,0.1,0.3,and0.5,

respectively,while k for pure TiO2was0.0002minà1and 0.00016minà1for P25.Therefore,the visible-light reactivity of TiO2was signi?cantly enhanced with these dopants,especially for CNS-0.3Fe-TiO2catalyst.The small but not negligible activity of pure TiO2and Degussa P25was attributed to the self-photosensitized process.[43]After absorbing light,the excited dyes such as Rhodamine B injected an electron into the conduction band of TiO2where it was captured by surface-adsorbed O2to form O2 à,and then,the dye cation radicals were degraded via attack by oxygen active species.However,the ef?ciency was very low because of the fairly slow interfacial electron transfer rate[43,44].In addition,it was noticed that the degradation of RB did not occur in the absence of catalysts or visible-light under the experimental conditions.

In order to explain the enhanced visible-light-activity of these multi-doped TiO2,several possible mechanisms were proposed.As shown in Fig.6,with the substitution for oxygen atoms by nonmetal atoms(carbon,nitrogen,and sulfur)and Ti4+by Fe3+in the crystal structure of TiO2,new impurity levels are introduced between the conduction and valence band of TiO2,then the electrons can be promoted to the conduction band from these impurity levels.The electrons can also be promoted from the valence band to another impurity level introduced by iron dopant, or from the lower to the higher impurity levels.Therefore,doped CNS-x Fe-TiO2photocatalysts have narrower band gap than pure TiO2and could increase the absorption in the visible-light region. Subsequently,the departed electrons and holes migrate to the surface of catalysts and react with adsorbed O2and H2O, respectively,forming O2 àand OH ,the main species responsible for the degradation of pollutants,such as RB in our case.With the addition of iron dopant,the reactivity of the catalyst is further increased.However,the reactivity decreases dramatically when x is increased from0.3to0.5wt%,indicating there is an optimal concentration of iron dopant.This is consistent with published data:[12]at concentration below the optimal value(0.3wt%in our case),there are fewer trapping sites available and Fe3+serves as shallow trapping sites for charge carrier(eàor h+),thereby separating the arrival time of eàand h+at the surface and increasing the ef?ciency.At high concentration,these trapped eàor h+might recombine together before migrating to the surface, resulting in lower photocatalytic activity of TiO2.Thus,the ef?ciency is strongly associated with Fe3+concentration.The optimal Fe3+dopant concentration in our case is not consistent with others,which might be related to different preparation methods,particle size,multiple dopants effect,or model com-pounds.The second mechanism is related with doped elemental carbon or carbonaceous species which could act as photosensitizer [21,22].As shown in Fig.7,under irradiation of visible-light,the excited photosensitizer injects electrons into the conduction band. The electrons could be further transferred to surface-adsorbed oxygen molecules and form O2 àand initiats the degradation of RB. Although this mechanism is similar to the dye self-photosensitized process we previously mentioned during the discussion of very low visible-light activity of pure TiO2or Degussa P25,its photo-ef?ciency should be higher because of higher interfacial electron transfer rate since it is the excited sensitizer rather than dye itself that injects an electron into the conduction band of TiO2after absorbing light.It was commonly accepted that dye was the only light absorbing species in self-photosensitized process[43]

Fig.5.The degradation of RB using different catalysts under visible-light

irradiation.

Fig.6.Schematic diagram of doped-TiO2and initial redox process after activation

light.

Fig.7.Schematic diagram of photosensitizer-TiO2system and initial redox process

after activation by light.

X.Yang et al./Applied Catalysis B:Environmental91(2009)657–662661

4.Conclusions

In this research,we successfully prepared multi-doped TiO2 photocatalysts with anatase structure.These multi-dopants,namely, carbon,nitrogen,sulfur,and iron retarded the growth and aggregation of TiO2particles.Multiple carbon species,substitutional and interstitial carbon atoms and carbonate species,were found in the lattice of TiO2.Nitrogen and sulfur atoms were incorporated into the lattice of TiO2and existed in the state of S2àand N2à,respectively, and iron dopant existed as Fe3+.These incorporations were veri?ed by XPS and XRD analyses.The diffuse re?ectance spectra suggested the photo absorption of multi-doped TiO2was extended to the visible-light region.It was assumed that these dopants introduced impurity levels between the conduction and valence band of TiO2, leading to narrower band gap and enhancing the visible-light https://www.wendangku.net/doc/9b7878318.html,pared with TiO2,these catalysts showed much higher activity for the degradation of RB under visible-light irradiation.Several possible mechanisms were proposed for the improvement of visible-light reactivity of multi-doped TiO2.

Acknowledgements

This work was supported by Army Research Of?ce(through DTRA contract SPO-AA06SP0012),the NanoScale Corporation,and the Kansas State University Targeted Excellence Program. References

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