Journal of Sol-Gel Science and Technology

, Volume 59, Issue 2, pp 352–357 | Cite as

Novel sulfur-doped niobium pentoxide nanoparticles: fabrication, characterization, visible light sensitization and redox charge transfer study

  • Mohammad Hossein Habibi
  • Reza Mokhtari
Original Paper


Novel sulfur-modified niobium(V) oxide nanoparticles (SNON) that firstly exhibited good visible light sensitization were fabricated by a modified sol–gel technique using a very stable sol containing niobium(V) chloride, oxalic acid, isopropanol as chelating agent and thiourea as sulfur source. The resulting S-doped Nb2O5 nanomaterials were characterized by cyclic voltammetry (CV), X-ray diffraction (XRD), energy-dispersive X-ray spectroscopy (EDAX), scanning electron microscope (SEM), ultra-violet diffuse reflectance (UV-DRS) and thermogravimetry thermal Analysis (TG-DTA). As against the response of unmodified niobium(V) oxide nanoparticles (UNON), the doped samples show different electrochemical response indicating an induced charge transfer across the niobium pentoxide/solution interface, thus forming two anodic peaks and a cathodic peak. This important observation was confirmed by UV-DRS in terms of band bending due to sulfur doping. Upon sulfur-modification, the absorption edge extends into the visible light region. The SEM observation shows that the SNPN existed in the mode of polycrystalline structure and the average grain size 63 nm. The EDAX analysis of undoped Nb2O5 and sulfur doped Nb2O5 shows the Nb2O5 (98%) and S (2%) content of nanopowder. These SNON nanoparticles are expected to be suitable candidates as visible light niobium(V) oxide nanoparticles sensitization.


Niobium(V) oxide Electrochemistry Sulfur-doped Redox charge transfer Nanoparticle 



The authors wish to thank the University of Isfahan for financially supporting this work.


  1. 1.
    Ge S, Jia H, Zhao H, Zheng Z, Zhang L (2010) First observation of visible light photocatalytic activity of carbon modified Nb2O5 nanostructures. J Mater Chem 20:3052–3058CrossRefGoogle Scholar
  2. 2.
    Li Y, Yan S, Qian L, Yang W, Xie Z, Chen Q, Yue B, He H (2006) Effect of tin on Nb2O5/α-Al2O3 catalyst for ethylene oxide hydration. J Catal 241:173–179CrossRefGoogle Scholar
  3. 3.
    Carniti P, Gervasini A, Biella S, Auroux A (2006) Niobic acid and niobium phosphate as highly acidic viable catalysts in aqueous medium: fructose dehydration reaction. Catal Today 118:373–378CrossRefGoogle Scholar
  4. 4.
    Yamashita K, Hirano M, Okumura K, Niwa M (2006) Activity and acidity of Nb2O5–MoO3 and Nb2O5–WO3 in the Friedel-Crafts alkylation. Catal Today 118:385–393CrossRefGoogle Scholar
  5. 5.
    de Paiva JB, Monteiro WR, Zacharias MA, Rodrigues JA, Cortez GG (2006) Characterization and catalytic behavior of MoO3/V2O5/Nb2O5 systems in isopropanol decomposition Braz. J Chem Eng 23:517–524Google Scholar
  6. 6.
    Prado AG, Bolzon LB, Pedroso CP, Moura AO, Costa LL (2008) Nb2O5 as efficient and recyclable photocatalyst for indigo carmine degradation. Appl Catal B 82:219–224CrossRefGoogle Scholar
  7. 7.
    Chen XY, Yu T, Fan XX, Zhang HT, Li ZS, Ye JH, Zou ZG (2007) Enhanced activity of mesoporous Nb2O5 for photocatalytic hydrogen production. Appl Surf Sci 253:8500–8508CrossRefGoogle Scholar
  8. 8.
    Esteves A, Oliveira LCA, Ramalho TC, Goncalves M, Anastacio AS, Carvalho HWP (2008) New materials based on modified synthetic Nb2O5 as photocatalyst for oxidation of organic contaminants. Catal Commun 10:330–332CrossRefGoogle Scholar
  9. 9.
    Saupe GB, Zhao Y, Bang J, Yesu NR, Carballo GA, Ordonez R, Bubphamala T (2005) Evaluation of a new porous titanium-niobium mixed oxide for photocatalytic water decontamination. Microchem J 81:156–162CrossRefGoogle Scholar
  10. 10.
    Xing JC, Shan ZC, Li KQ, Bian JJ, Lin XP, Wang WD, Huang FQ (2008) Photocatalytic activity of Nb2O5/SrNb2O6 heterojunction on the degradation of methyl orange. J Phys Chem Solids 69:23–28CrossRefGoogle Scholar
  11. 11.
    Lin HY, Huang HC, Wang WL (2008) Preparation of mesoporous In–Nb mixed oxides and its application in photocatalytic water splitting for hydrogen production. Microporous Mesoporous Mater 115:568–575CrossRefGoogle Scholar
  12. 12.
    Torres JD, Faria EA, SouzaDe JR, Prado AGS (2006) Preparation of photoactive chitosan–niobium (V) oxide composites for dye degradation. J Photochem Photobiol A 182:202–206CrossRefGoogle Scholar
  13. 13.
    Prado AGS, Faria EA, SouzaDe JR, Torres JD (2005) Ammonium complex of niobium as a precursor for the hydrothermal preparation of cellulose acetate/Nb2O5 photocatalyst. J Mol Catal A: Chem 237:115–119CrossRefGoogle Scholar
  14. 14.
    Matsui H, Kira K, Karuppuchamy S, Yoshihara M (2009) The electronic behaviors of visible light sensitive Nb2O5/Cr2O3/carbon clusters composite materials. Curr Appl Phys 9:592–597CrossRefGoogle Scholar
  15. 15.
    Habibi MH, Nasr-Esfahani M (2008) Silver doped TiO2 nanostructure composite photocatalyst film synthesized by sol–gel spin and dip coating technique on glass. Int J Photoenergy ID:628713Google Scholar
  16. 16.
    Habibi MH, Vosoghian H (2005) Photocatalytic degradation of some organic sulfides as environmental pollutants using titanium dioxide suspension. J Photochem Photobiol A: Chem 172:45–52CrossRefGoogle Scholar
  17. 17.
    Habibi MH, Hassanzadeh A, Mahdavi S (2005) The effect of operational parameters on the photocatalytic degradation of three textile azo dyes in aqueous TiO2 suspensions. J Photochem Photobiol A: Chem 172:89–96CrossRefGoogle Scholar
  18. 18.
    Habibi MH, Talebian N (2006) Characterization and photocatalytic activity of nanostructured indium tin oxide thin-film electrode for azo-dye degradation. Thin Solid Films 515:1461–1469CrossRefGoogle Scholar
  19. 19.
    Habibi MH, Talebian N, Choi JH (2007) The effect of annealing on photocatalytic properties of nanostructured titanium dioxide thin films. Dyes Pigm 73:103–110CrossRefGoogle Scholar
  20. 20.
    Habibi MH, Talebian N (2007) Photocatalytic degradation of an azo dye X6G in water: a comparative study using nanostructured indium tin oxide and titanium oxide thin films. Dyes Pigm 73:186–194CrossRefGoogle Scholar
  21. 21.
    Kominami H, Oki K, Kohno M, Onoue SI, Kera Y, Ohtani B (2001) Novel solvothermal synthesis of Niobium(V) oxide powders and their photocatalytic activity in aqueous suspensions. J Mater Chem 11:604–609CrossRefGoogle Scholar
  22. 22.
    Tsuzuki T, McCormick PG (2001) Mechanochemical synthesis of niobium pentoxide nanoparticles mater. Trans 42:1623–1628Google Scholar
  23. 23.
    Campos EA, Gushikem Y (1997) Composite membrane of Niobium(V) oxide and cellulose acetate: preparation and characterization. J Coll Interface Sci 193:121–129CrossRefGoogle Scholar
  24. 24.
    Sayama K, Sugihara H, Arakawa H (1998) Photoelectrochemical properties of a porous Nb2O5 electrode sensitized by a ruthenium dye. Chem Mater 10:3825–3830CrossRefGoogle Scholar
  25. 25.
    Yamazaki M, Kojima K, Shiraishi H, Maegawa A (1997) Observation of green upconversion fluorescence in Er3+ doped Nb2O5 prepared by the sol–gel method. Phys Chem Glasses 38:246–247Google Scholar
  26. 26.
    Catauro M, Pagliuca C, Lisi L, Ruoppolo G (2002) Synthesis of alkoxide-derived V-Nb catalysts prepared by sol–gel route. Thermochim Acta 381:65–67CrossRefGoogle Scholar
  27. 27.
    Ristic M, Popovic S, Music S (2004) Sol–gel synthesis and characterization of Nb2O5 powders. Mater Lett 58:2658–2663CrossRefGoogle Scholar
  28. 28.
    Reddy KM, Baruwati B, Jayalakshmi M, Rao MM, Manorama SV (2005) S-, N- and C-doped titanium dioxide nanoparticles: synthesis, characterization and redox charge transfer study. J Solid State Chem 178:3352–3358CrossRefGoogle Scholar
  29. 29.
    Habibi MH, Kamrani R, Mokhtari R (2010) Fabrication and characterization of copper nanoparticles using thermal reduction: the effect of nonionic surfactants on size and yield of nanoparticles. Microchim Acta 171:91–95CrossRefGoogle Scholar
  30. 30.
    Habibi MH, Zendehdel M (2010) Fabrication and characterization of self-assembled multilayer nanostructure titania with high preferential (101) orientation on alumina thin films using layer by layer dip-coating method. Current Nanoscience 6:642–647CrossRefGoogle Scholar
  31. 31.
    Aegerter MA (2001) Sol–gel niobium pentoxide: a promising material for electrochromic coatings, batteries, nanocrystalline solar cells and catalysis. Sol Energy Mater Sol Cells 68:401–422CrossRefGoogle Scholar
  32. 32.
    Parthasarathy M, Ramgir NS, Sathe BR, Mulla IS, Pillai VK (2007) Surface-state-mediated electron transfer at nanostructured ZnO multipod/electrolyte interfaces. J Phys Chem C 111:13092–13102CrossRefGoogle Scholar
  33. 33.
    Hamann TW, Gstrein F, Brunschwig BS, Lewis NS (2005) Measurement of the free energy dependence of interfacial charge-transfer rate constants using ZnO/H2O semiconductor/liquid contacts. J Am Chem Soc 127:7815–7824CrossRefGoogle Scholar
  34. 34.
    Barros Filho DA, Abreu filho PP, Werner U, Aegerter MA (1997) Photoelectrochemical properties of sol–gel Nb2O5 films. J Sol–Gel Sci Technol 8:735–742Google Scholar
  35. 35.
    Lindgren T, Mwabora JM, Avedano E, Jonsson J, Hoel A, Granquist CG, Lindquist SE (2003) Photoelectrochemical and optical properties of nitrogen doped titanium dioxide films prepared by reactive DC magnetron sputtering. J Phys Chem B 107:5709–5716CrossRefGoogle Scholar
  36. 36.
    Santiago FF, Mora-Sero I, Garcia-Belmonte G, Bisquert J (2003) Cyclic voltammetry studies of nanoporous semiconductors. Capacitive and reactive properties of nanocrystalline TiO2 electrodes in aqueous electrolyte. J Phys Chem B 107:758–768CrossRefGoogle Scholar
  37. 37.
    Provenzano PL, Jindal GR, Sweet JR, White WB (2001) Flame excited luminescence in the oxides Ta2O5, Nb2O5, TiO2, ZnO, and SnO2. J Lumin 92:297–305CrossRefGoogle Scholar
  38. 38.
    Prado AGS, Bolzon LB, Pedroso CP, Moura AO, Costa LL (2008) Nb2O5 as efficient and recyclable photocatalyst for indigo carmine degradation. Appl Catal B: Environ 82:219–224CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media, LLC 2011

Authors and Affiliations

  1. 1.Nanotechnology Laboratory, Department of ChemistryUniversity of IsfahanIsfahanI.R. Iran

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