Abstract
The high purity γ-Ti3O5 thin films deposited on single-crystal SiO2 substrates are firstly prepared via sol–gel method combined with hydrogen reduction processing. In this reported work, the influences of reduction of temperature, hydrogen flow rate and holding time on the reduced phases are investigated. The as-prepared materials are characterized by glancing incident angle X-ray diffraction, scanning electron microscopy. Based on the results of single factor and orthogonal tests, the optimum condition for synthesizing high purity Ti3O5 thin films are as follows: the hydrogen gas flow rate is 0.8 L min−1, the reduction temperature is 1150 °C and the holding time is 1 h. Temperature dependence of PXRD patterns and electrical conductivity (σ) variation demonstrates that the temperature of phase transition between monoclinic I2/c crystal structure of γ-Ti3O5 thin film and monoclinic P2/a crystal structure of δ-Ti3O5 thin film was 225 K. The four-point probe test shows that the room-temperature conductivity of γ-Ti3O5 thin film is 202.1 S m−1.
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References
L. Zheng, The preparation and oxygen-sensing properties of α-Ti3O5 thin film. Sens. Actuators B 88, 115–119 (2003)
D. Wei, W. Huang, Q. Shi, T. Lu, B. Huang, Effect of coating layers on nano-TiO2 particles on the preparation of nanocrystalline λ-Ti3O5 by carbonthermal reduction. J. Mater. Sci. 27, 4216–4222 (2016)
L. Kotsedi, Z.Y. Nuru, S.M. Eaton, F.R. Cummings, S. Lo Turco, O.M. Ntwaeaborwa, R. Ramponi, M. Maaza, Titanium oxide nanocoating on a titanium thin film deposited on a glass substrate. Thin Solid Films 603, 446–451 (2016)
Y. Wu, Q. Zhang, X. Wu, S. Qin, J. Liu, High pressure structural study of β-Ti3O5: X-ray diffraction and Raman spectroscopy. J. Solid State Chem. 192, 356–359 (2012)
E. Vallejo, D. Olguin, New metastable phases in a trititanium pentoxide compound. Mater. Res. Express. 2, 126101 (2015)
M. Onoda, Phase Transitions of Ti3O5. J. Solid State Chem. 136, 67–73 (1998)
K. Tanaka, T. Nasu, Y. Miyamoto, N. Ozaki, S. Tanaka et al., Structural phase transition between γ-Ti3O5 and δ-Ti3O5 by breaking of a one-dimensionally conducting pathway. Cryst. Growth Des. 15, 653–657 (2014)
H. Tokoro, M. Yoshikiyo, K. Imoto, A. Namai, T. Nasu, K. Nakagawa, N. Ozaki, F. Hakoe, K. Tanaka, K. Chiba, R. Makiura, K. Prassides, S.-I. Ohkoshi, External stimulation-controllable heat-storage ceramics. Nat. Commun. 6, 7037 (2015)
R. Makiura, Y. Takabayashi, A.N. Fitch, H. Tokoro, S. Ohkoshi, K. Prassides, Nanoscale effects on the stability of the λ-Ti3O5 polymorph. Supporting Information, Chem. Asian J. 6, 1886–1890 (2011)
S.-I. Ohkoshi, Y. Tsunobuchi, T. Matsuda, K. Hashimoto, A. Namai, F. Hakoe, H. Tokoro, Synthesis of a metal oxide with a room-temperature photoreversible phase transition. Nat. Chem. 2, 539–545 (2010)
S. Åsbrink, A. Magnéli, Crystal structure studies on trititanium pentoxide, Ti3O5. Acta Crystallogr. 12, 575–581 (1959)
H. Iwasaki, N. Bright, J. Rowland, The polymorphism of the oxide Ti3O5. J. Less Common Metals 17, 99–110 (1969)
S.-H. Hong, S. Åsbrink, The structure of γ- Ti3O5 at 297 K. Acta Crystallogr. Sect. B. 38, 2570–2576 (1982)
R. Zhu, Y. Liu, J. Ye, X. Zhang, Magnéli phase Ti4O7 powder from carbothermal reduction method: Formation, conductivity and optical properties. J. Mater. Sci. 24, 4853–4856 (2013)
Y. Chen, J. Mao, Sol–gel preparation and characterization of black titanium oxides Ti2O3 and Ti3O5. J. Mater. Sci. 25, 1284–1288 (2014)
Z. Ertekin, U. Tamer, K. Pekmez, Cathodic electrochemical deposition of Magnéli phases TinO2n–1 thin films at different temperatures in acetonitrile solution. Electrochim. Acta 163, 77–81 (2015)
C. Hauf, R. Kniep, G. Pfaff, Preparation of various titanium suboxide powders by reduction of TiO2 with silicon. J. Mater. Sci 34, 1287–1292 (1999)
T. Nasu, H. Tokoro, K. Tanaka, F. Hakoe, A. Namai, S.I. Ohkoshi, Sol–gel synthesis of nanosized λ-Ti3O5 crystals. IOP Conf. Ser. 54, 012008 (2014)
N. Stem, M.L. De Souza, D.L.A. De Faria, S.G. Dos Santos Filho, Formation of Ti(III) and Ti(IV) states in Ti3O5 nano- and microfibers obtained from hydrothermal annealing of C-doped TiO2 on Si. Thin Solid Films 558, 67–74 (2014)
G. Asbrink, S. Åsbrink, A. Magnéli, H. Okinaka, K. Kosuge, S. Kachi, A Ti3O5 modification of V3O5-type structure. Acta Chem. Scand. 25, 3889–3890 (1971)
Y. Chen, J. Mao, Reduced titanium oxide Ti3O5 powder as a promising conductive additive for LiFePO4-based lithium-ion batteries. J. Mater. Sci. 25, 5153–5157 (2014)
G. Liu, W.-X. Huang, Y. Yi, Preparation and Optical Storage Properties of λ-Ti3O5 Powder. J. Inorg. Mater. 28, 425–430 (2013)
M. Nazari, Y. Zhao, V. V. Kuryatkov, Z.Y. Fan, A.A. Bernussi, M. Holtz, Temperature dependence of the optical properties of VO2 deposited on sapphire with different orientations. Phys. Rev. B 87, 1–7 (2013)
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This work was financially supported by the National Natural Science Foundation of China (No. 61271075).
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Huang, B., Huang, W., Shi, Q. et al. The preparation and phase transformation characteristics of γ-Ti3O5 thin film. J Mater Sci: Mater Electron 28, 7868–7873 (2017). https://doi.org/10.1007/s10854-017-6484-7
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DOI: https://doi.org/10.1007/s10854-017-6484-7