Journal of Sol-Gel Science and Technology

, Volume 67, Issue 2, pp 288–296 | Cite as

Monodispersed titanium oxide nanoparticles in N,N-dimethylformamide: water solutions

  • Hélène Terrisse
  • Audry-Fred Bando
  • Thomas Cottineau
  • Luc Brohan
  • Mireille Richard-Plouet
Original Paper
First Online:
Received:
Accepted:

Abstract

Because of both its complexing ability toward Ti cations and reactivity in highly acidic medium, N,N-dimethylformamide (DMF) can be used to control the hydrolysis and condensation of Titanium oxide frameworks, starting from Ti oxychloride as precursor. The addition of water allows promotion of hydrolysis of the aldehyde while controlling the size of the nanoparticles formed in the solution. The as-prepared colloidal solutions are very stable, up to 3 months, depending on the initial titanium concentration, the DMF/Water ratio, and the thermal treatment. The sol to gel transformation was monitored by viscosimetry measurements as a function of ageing time and heat treatment temperature. Optimization of pre-treatment at moderate temperature leads to fine control over the gelation process.

Keywords

TiO2 colloids Nanoparticles Polycondensation Dynamic light scattering Viscosity Sol–gel transition 
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Notes

Acknowledgments

The authors gratefully thank Dr. Jason Cody for reading the manuscript.

Supplementary material

10971_2013_3078_MOESM1_ESM.doc (46 kb)
Supplementary material 1 (DOC 46 kb)
10971_2013_3078_MOESM2_ESM.doc (42 kb)
Supplementary material 2 (DOC 42 kb)
10971_2013_3078_MOESM3_ESM.doc (108 kb)
Supplementary material 3 (DOC 108 kb)

References

  1. 1.
    Oh H, Krantz J, Litzov I, Stubhan T, Pinna L, Brabec CJ (2011) Comparison of various sol-gel derived metal oxide layers for inverted organic solar cells. Sol Energy Mater Sol Cells 95:2194–2199CrossRefGoogle Scholar
  2. 2.
    Stubhan T, Oh H, Pinna L, Krantz J, Litzov I, Brabec CJ (2011) Inverted organic solar cells using a solution processed aluminum-doped zinc oxide buffer layer. Org Electron 12:1539–1543CrossRefGoogle Scholar
  3. 3.
    Lou SJ, Szarko JM, Xu T, Yu L, Marks TJ, Chen LX (2011) Effects of additives on the morphology of solution phase aggregates formed by active layer components of high-efficiency organic solar cells. J Am Chem Soc 133:20661–20663CrossRefGoogle Scholar
  4. 4.
    Baes CF, Mesmer RE (1976) The hydrolysis of cations. New York, WileyGoogle Scholar
  5. 5.
    Haruta M, Delmon B (1986) Preparation of homodisperse solids. J Chim Phys Phys Chim Biol 83:859–868Google Scholar
  6. 6.
    Jolivet JP, Henry M, Livage J, Bescher EP (2003) Metal oxide chemistry and synthesis: from solution to solid state. Wiley, ChichesterGoogle Scholar
  7. 7.
    Jolivet JP, Cassaignon S, Chaneac C, Chiche D, Tronc E (2008) Design of oxide nanoparticles by aqueous chemistry. J Sol Gel Sci Technol 46:299–305CrossRefGoogle Scholar
  8. 8.
    Jolivet JP, Cassaignon S, Chaneac C, Chiche D, Durupthy O, Portehault D (2010) Design of metal oxide nanoparticles: control of size, shape, crystalline structure and functionalization by aqueous chemistry. C R Chim 13:40–51CrossRefGoogle Scholar
  9. 9.
    Mutin PH, Vioux A (2009) Nonhydrolytic processing of oxide-based materials: simple routes to control homogeneity, morphology, and nanostructure. Chem Mater 21:582–596CrossRefGoogle Scholar
  10. 10.
    Vioux A (1997) Nonhydrolytic sol–gel routes to oxides. Chem Mater 9:2292–2299CrossRefGoogle Scholar
  11. 11.
    Debecker DP, Mutin PH (2012) Non-hydrolytic sol–gel routes to heterogeneous catalysts. Chem Soc Rev 41:3624–3650CrossRefGoogle Scholar
  12. 12.
    Debecker DP, Hulea V, Mutin PH (2013) Mesoporous mixed oxide catalysts via non-hydrolytic sol–gel: a review. Appl Catal A 451:192–206CrossRefGoogle Scholar
  13. 13.
    Niederberger N (2007) Nonaqueous sol–gel routes to metal oxide nanoparticles. Acc Chem Res 40:793–800CrossRefGoogle Scholar
  14. 14.
    Djerdj I, Arcon D, Jaglicic Z, Niederberger N (2008) Nonaqueous synthesis of metal oxide nanoparticles: short review and doped titanium dioxide as case study for the preparation of transition metal-doped oxide nanoparticles. J Solid State Chem 181:1571–1581CrossRefGoogle Scholar
  15. 15.
    Garnweitner G, Niederberger M (2008) Organic chemistry in inorganic nanomaterials synthesis. J Mater Chem 18:1171–1182CrossRefGoogle Scholar
  16. 16.
    Pinna N, Niederberger M (2008) Surfactant-free nonaqueous synthesis of metal oxide nanostructures. Angew Chem Int Ed 47:5292–5304CrossRefGoogle Scholar
  17. 17.
    Bilecka I, Niederberger M (2010) New developments in the nonaqueous and/or non-hydrolytic sol–gel synthesis of inorganic nanoparticles. Electrochim Acta 55:7717–7725CrossRefGoogle Scholar
  18. 18.
    Songyuan Dai JW, Sui Y, Shi C, Huang Y, Chen S, Pan X, Fang X, Hu L, Kong F, Wang K (2004) Dye-sensitized solar cells, from cell to module. Sol Energy Mater Sol Cells 84:125–133CrossRefGoogle Scholar
  19. 19.
    Kim JJSS, Chun C, Hong JC, Kim DY (2007) Hybrid solar cells with ordered TiO2 nanostructures and MEH-PPV. J Photochem Photobiol, A 188:364–370CrossRefGoogle Scholar
  20. 20.
    Slooff MMWLH, Kroon JM (2004) Hybrid TiO2: polymer photovoltaic cells made from a titanium oxide precursor. Thin Solid Films 451–452:634–638CrossRefGoogle Scholar
  21. 21.
    Gomez EMM, Olsson E, Hagfeldt A, Lindquist SE, Granqvist CG (2000) Nanocrystalline Ti-oxide-based solar cells made by sputter deposition and dye sensitization: efficiency versus film thickness. Sol Energy Mater Sol Cells 62:259–263CrossRefGoogle Scholar
  22. 22.
    Beuvier T, Richard-Plouet M, Mancini-Le Granvalet M, Brousse T, Crosnier O, Brohan L (2010) TiO2(B) nanoribbons as negative electrode material for lithium ion batteries with high rate performance. Inorg Chem 49:8457–8464CrossRefGoogle Scholar
  23. 23.
    Liu S, Jia H, Han L, Wang J, Gao P, Xu D, Yang J, Che S (2012) Nanosheet-constructed porous TiO2-B for advanced lithium ion batteries. Adv Mater 24:3201–3204CrossRefGoogle Scholar
  24. 24.
    Yoon S, Lee ES, Manthiram A (2012) Microwave-solvothermal synthesis of various polymorphs of nanostructured TiO2 in different alcohol media and their lithium ion storage properties. Inorg Chem 51:3505–3512CrossRefGoogle Scholar
  25. 25.
    Nguyen Nang D, Nguyen Minh Q, Do Ngoc C, Zikova M, Truong VV (2011) Highly-efficient electrochromic performance of nanostructured TiO2 films made by doctor blade technique. Sol Energy Mater Sol Cells 95:618–623CrossRefGoogle Scholar
  26. 26.
    Pan JH, Zhao XS, Lee WI (2011) Block copolymer-templated synthesis of highly organized mesoporous TiO2-based films and their photoelectrochemical applications. Chem Eng J 170:363–380CrossRefGoogle Scholar
  27. 27.
    Song YY, Gao ZD, Wang JH, Xia XH, Lynch R (2011) Multistage coloring electrochromic device based on TiO2 nanotube arrays modified with WO3 nanoparticles. Adv Funct Mater 21:1941–1946CrossRefGoogle Scholar
  28. 28.
    Fujishima A, Rao TN, Tryk DA (2000) Titanium dioxide photocatalysis. J Photochem Photobiol, C 1:1–21CrossRefGoogle Scholar
  29. 29.
    Fujishima A, Zhang X (2006) Titanium dioxide photocatalysis: present situation and future approaches. C R Chim 9:750–760CrossRefGoogle Scholar
  30. 30.
    Addamo VAM, Paola AD, García-López E, Loddo V, Marcì G, Palmisano L (2008) Photocatalytic thin films of TiO2 formed by a sol–gel process using titanium tetraisopropoxide as the precursor. Thin Solid Films 516:3802–3807CrossRefGoogle Scholar
  31. 31.
    Kitano M, Ueshima M, Anpo M (2007) Recent developments in titanium oxide-based photocatalysts. App Catal A 325:1–14CrossRefGoogle Scholar
  32. 32.
    Chung-Shin Lu FDM, Wu CW, Wu RJ, Chen CC (2008) Titanium dioxide-mediated photocatalytic degradation of acridine orange in aqueous suspensions under UV irradiation. Thin Solid Films 516:3802–3807CrossRefGoogle Scholar
  33. 33.
    Mardare D, Iftimie N, Luca D (2008) TiO2 thin films as sensing gas materials. J Non Cryst Solids 354:4396–4400CrossRefGoogle Scholar
  34. 34.
    Laugel N, Ladhari N, Arntz Y, Gonthier E, Haikel Y, Voegel JC, Schaaf P, Ball V (2008) Composite films of polycations and TiO2 nanoparticles with photoinduced superhydrophilicity. J Colloid Interface Sci 324:127–133CrossRefGoogle Scholar
  35. 35.
    Sakai N, Watanabe T, Hashimoto K (2001) Enhancement of the photoinduced hydrophilic conversion rate of TiO2 film electrode surfaces by anodic polarization. J Phys Chem B 105(15):3023–3026CrossRefGoogle Scholar
  36. 36.
    Gao Y, Koumoto K (2004) Light-excited superhydrophilicity of amorphous TiO2 thin films deposited in an aqueous peroxotitanate solution. Langmuir 20:3188–3194CrossRefGoogle Scholar
  37. 37.
    Cottineau T, Richard-Plouet M, Rouet A, Puzenat E, Sutrisno H, Piffard Y, Petit PE, Brohan L (2008) Photosensitive titanium oxo-polymers: synthesis and structural characterization. Chem Mater 20:1421–1430CrossRefGoogle Scholar
  38. 38.
    Pecora R (2000) Dynamic light scattering measurement of nanometer particles in liquids. J Nanopart Res 2:123–131CrossRefGoogle Scholar
  39. 39.
    Kaszuba M, McKnight D, Connah MT, McNeil-Watson FK, Nobbmann U (2008) Measuring sub nanometre sizes using dynamic light scattering. J Nanopart Res 10:823–829CrossRefGoogle Scholar
  40. 40.
    Challis BC, Jones SP (1974) Acid-catalyzed decomposition of N-nitroso-2-pyrrolidone. Rare example of amide hydrolysis via SN2 displacement on N-conjugate acid. J Chem Soc Chem Commun 18:748–749Google Scholar
  41. 41.
    Challis BC, Jones SP (1975) Chemistry of nitroso-compounds. 9. General acid-catalyzed decomposition of N-nitroso-2-pyrrolidone, an example of amide hydrolysis via SN2 displacement on N-conjugate acid. J Chem Soc Perkin Trans 2:153–160Google Scholar
  42. 42.
    Challis BC, Jones SP (1979) Chemistry of nitroso-compounds. 13. Decomposition of N-nitroso-2-pyrrolidone under basic conditions, an unusual example of nucleophilic catalyzed-hydrolysis of an amide derivative. J Chem Soc Perkin Trans 2:703–706Google Scholar
  43. 43.
    Cottineau T, Richard-Plouet M, Mevellec JY, Brohan L (2011) Hydrolysis and complexation of N, N-dimethylformamide in new nanostructurated titanium oxide hybrid organic–inorganic sols and gel. J Phys Chem C 115:12269–12274CrossRefGoogle Scholar
  44. 44.
    Pattier B, Henderson M, Brotons G, Gibaud A (2010) Study of titanium oxide sol–gel condensation using small angle X-ray scattering. J Phys Chem B 114:5227–5232CrossRefGoogle Scholar
  45. 45.
    Nemethy G, Scheraga HA (1962) Structure of water and hydrophobic bonding in proteins. 1. A model for thermodynamic properties of liquid water. J Chem Phys 36:3382–3388CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media New York 2013

Authors and Affiliations

  • Hélène Terrisse
    • 1
  • Audry-Fred Bando
    • 1
  • Thomas Cottineau
    • 1
    • 2
  • Luc Brohan
    • 1
  • Mireille Richard-Plouet
    • 1
  1. 1.Institut des Matériaux Jean Rouxel (IMN)Université de Nantes, CNRSNantes cedex 3France
  2. 2.Institut de Chimie et Procédés pour l’Energie l’Environnement et la Santé (ICPEES)Université de Strasbourg/CNRSStrasbourgFrance

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