Abstract
TiO2− x N y film has been synthesized successfully through the sol-gel method. It is found that the anatase phase is formed at 400 °C and converted to rutile phase at 600 °C. The response surface methodology (RSM) and Box-Behnken design were employed to optimize the process conditions of sol-gel process. Based on the results in preliminary experiments, we selected molar ratio of surfactant to Ti, molar ratio of acetylacetone to Ti, molar ratio of water to Ti and calcination temperature as the key process factors affecting the roughness of TiO2− x N y film. The adjusted determination coefficient (R Adj 2) of the regression model was 0.9651, which indicated that the regression model is significant. By analysing the contour plots of response surface as well as solving the regression model, the optimized conditions were obtained as: 0.19 for molar ratio of surfactant to Ti, 2.01 for molar ratio of acetylacetone to Ti, 1.38 for molar ratio of water to Ti and 500 °C for calcination temperature. The predicted roughness of TiO2− x N y film for the optimized condition was calculated to be 41 nm. Confirmation experiments using the optimized conditions were performed, and a value about 43 nm was obtained. The experimental results are in good agreement with the predicted results.
This is a preview of subscription content, log in via an institution to check access.
Similar content being viewed by others
References
Algueró M, Calzada M L, Quintana C and Pardo L 1999 Appl. Phys. A68 583
Asahi R, Morikawa T, Ohwaki T, Aoki K and Taga Y 2001 Science 293 269
Box G E P and Behnken D W 1960 Technometrics 2 455
Box G E P and Draper N R 1987 Empirical model-building and response surfaces (New York: John Wiley & Sons)
Fujishima A and Honda K 1972 Nature 238 37
Hsieh C S and Liou T S 2001 Qual. Eng. 13 449
Irie H, Watanabe Y and Hashimoto K 2003 J. Phys. Chem. B107 5483
Jang H K, Whangbo S W, Kim H B, Im K Y, Lee Y S, Lyo I W, Whang C N, Kim G, Lee H S and Lee J M 2000 J. Vac. Sci. Technol., A, Vac. Surf. Films 18 917
Lindgren T, Mwabora J M, Avendano E and Jonsson J 2003 J. Phys. Chem. B107 5709
Linsebigler A L, Lu G Q and Yates J T 1995 Chem. Rev. 95 735
Montgomery D C 2001 (New York: John Wiley & Sons)
Moon J, Suvaci E, Li T, Costantino A and Adair J H 2002 J. Eur. Ceram. Soc. 22 809
Morgenthaler S and Schumacher M M 1999 Chemom. Intell. Lab. Syst. 47 127
Myers R H and Montgomery D C 1995 Response surface methodology: process and product optimization using designed experiments (New York: John Wiley & Sons)
Nakamura I, Negishi N, Kutsuna S, Ihara T, Sugihara S and Takeuchi K 2000 J. Mol. Catal. A: Chem. 161 205
Saha N C and Tompkins H G 1992 J. Appl. Phys. 72 3072
Selvaraj U, Prasadarao A V and Komarneni S 1994 Mater. Lett. 20 71
Shankar K, Tep K C, Mor G K and Grimes C A 2006 J. Phys. D: Appl. Phys. 39 2361
So W W, Park S B, Kim K J, Shin C H and Moon S J 2001 J. Mater. Sci. 36 4299
Sreekantan S, Hazan R and Lockman Z 2009 Thin Solid Films 518 16
Syoufian A and Nakashima K 2007 J. Coll. Interf. Sci. 313 213
Vitiello R P, Macak J M, Ghicov A and Tsuchiya H 2006 Electrochem. Commun. 8 544
Yang W D and Hung K M 2002 J. Mater. Sci. 37 1337
Yang T S, Shu C B and Wong M S 2004 Surf. Sci. 548 75
Yuan J, Chen M, Shi J and Shangguan W 2006 Int. J. Hydrogen Energy 31 1326
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Liu, R., Hsieh, CS., Yang, WD. et al. Optimization of process conditions for the production of TiO2− x N y film by sol-gel process using response surface methodology. Bull Mater Sci 37, 1301–1308 (2014). https://doi.org/10.1007/s12034-014-0075-5
Received:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s12034-014-0075-5