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Systematic variation of preparation time, temperature, and pressure in hydrothermal synthesis of macro-/mesoporous TiO2 for photocatalytic air treatment


Systematic variation of preparation time, temperature, and pressure in hydrothermal synthesis of macro-/mesoporous TiO2 for photocatalytic air treatment

Haghighat, Fariborz, Mamaghani, Alireza Haghighat and Lee, Chang-Seo (2019) Systematic variation of preparation time, temperature, and pressure in hydrothermal synthesis of macro-/mesoporous TiO2 for photocatalytic air treatment. Journal of Photochemistry and Photobiology A: Chemistry . ISSN 10106030 (In Press)

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Official URL: http://dx.doi.org/10.1016/j.jphotochem.2019.04.022


A series of porous TiO2 photocatalysts are prepared, by systematically varying the preparation conditions (time, temperature, or pressure (i.e. filling ratio)), characterized, and evaluated in photocatalytic oxidation of toluene and methyl ethyl ketone (MEK) to explore preparation-property-performance relationships. A detailed characterization has been conducted via X-ray diffraction (XRD), N2 adsorption-desorption, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier transform infrared (FTIR), and UV-vis spectroscopy. Furthermore, hydroxyl radical (•OH) generation on the surface of TiO2 is measured by a photoluminescence (PL) method using terephthalic acid (TA) as probe molecule. All the hydrothermally-prepared samples possessed good crystallinity (79.5-89 %), large surface area (134.9-237.2 m2/g), small crystal size (5.9-10 nm), and mesoporous structure. SEM images revealed presence of macropores and marcochannels, and N2 adsorption-desorption and TEM analyses indicated a significant amount of mesopores. PL and XRD results demonstrated a good proportionality between surface area normalized •OH generation and crystallinity. The complex interplay among various properties (especially crystallinity and surface area) led to appearance of activity optimums. Photocatalyst prepared at 12 h, 200 °C, and 80% filling ratio exhibited the best toluene and MEK removal efficiencies, which surpass those of P25 by factors of 2.08 and 1.85 times, respectively. The superior photocatalytic activity of developed TiO2 catalysts might be attributed to high surface area and existence of meso-/macropores that provide a large number of active sites, and facilitate light penetration and pollutants diffusion. The presented property-activity relationships can be utilized as potential design criteria for the development of new TiO2 photocatalysts for air purification.

Divisions:Concordia University > Gina Cody School of Engineering and Computer Science > Building, Civil and Environmental Engineering
Item Type:Article
Authors:Haghighat, Fariborz and Mamaghani, Alireza Haghighat and Lee, Chang-Seo
Journal or Publication:Journal of Photochemistry and Photobiology A: Chemistry
Digital Object Identifier (DOI):10.1016/j.jphotochem.2019.04.022
Keywords:Photocatalytic oxidation (PCO); Titanium dioxide (TiO2); Hydrothermal; Hydroxyl radical; Photoluminescence; Air purification
ID Code:985326
Deposited By: ALINE SOREL
Deposited On:29 Apr 2019 16:18
Last Modified:29 Apr 2019 16:18


A. Fujishima, K. Honda. Electrochemical Photolysis of Water at a Semiconductor Electrode, Nature, 238 (1972), p. 37

A. Di Paola, E. García-López, G. Marcì, L. Palmisano. A survey of photocatalytic materials for environmental remediation, Journal of Hazardous Materials, 211-212 (2012), pp. 3-29

C. Yu, W. Zhou, H. Liu, Y. Liu, D.D. Dionysiou. Design and fabrication of microsphere photocatalysts for environmental purification and energy conversion, Chemical Engineering Journal, 287 (2016), pp. 117-129

R.A.R. Monteiro, A.M.T. Silva, J.R.M. Ângelo, G.V. Silva, A.M. Mendes, R.A.R. Boaventura, V.J.P. Vilar. Photocatalytic oxidation of gaseous perchloroethylene over TiO2 based paint, Journal of Photochemistry and Photobiology A: Chemistry, 311 (2015), pp. 41-52

A.H. Mamaghani, F. Haghighat, C.-S. Lee. Photocatalytic oxidation technology for indoor environment air purification: The state-of-the-art, Applied Catalysis B: Environmental, 203 (2017), pp. 247-269

A.H. Mamaghani, F. Haghighat, C.-S. Lee. Photocatalytic degradation of VOCs on various commercial titanium dioxides: Impact of operating parameters on removal efficiency and by-products generation, Building and Environment, 138 (2018), pp. 275-282

M. Sboui, S. Bouattour, L.F. Liotta, V.L. Parola, M. Gruttadauria, G. Marcì, S. Boufi. Paper-TiO2 composite: An effective photocatalyst for 2-propanol degradation in gas phase, Journal of Photochemistry and Photobiology A: Chemistry, 350 (2018), pp. 142-151

X. Chen, S.S. Mao. Titanium Dioxide Nanomaterials: Synthesis, Properties, Modifications, and Applications, Chemical Reviews, 107 (2007), pp. 2891-2959

M. Ouzzine, M.A. Lillo-Ródenas, A. Linares-Solano. Photocatalytic oxidation of propene in gas phase at low concentration by optimized TiO2 nanoparticles, Applied Catalysis B: Environmental, 134-135 (2013), pp. 333-343

A. Bazyari, A.A. Khodadadi, A. Haghighat Mamaghani, J. Beheshtian, L.T. Thompson, Y. Mortazavi. Microporous titania–silica nanocomposite catalyst-adsorbent for ultra-deep oxidative desulfurization, Applied Catalysis B: Environmental, 180 (2016), pp. 65-77

A. Alonso-Tellez, R. Masson, D. Robert, N. Keller, V. Keller. Comparison of Hombikat UV100 and P25 TiO2 performance in gas-phase photocatalytic oxidation reactions, Journal of Photochemistry and Photobiology A: Chemistry, 250 (2012), pp. 58-65

Y. Zhu, T. Mei, Y. Wang, Y. Qian. Formation and morphology control of nanoparticlesvia solution routes in an autoclave, Journal of Materials Chemistry, 21 (2011), pp. 11457-11463

K. Byrappa, T. Adschiri. Hydrothermal technology for nanotechnology, Progress in Crystal Growth and Characterization of Materials, 53 (2007), pp. 117-166

A.H. Mamaghani, F. Haghighat, C.-S. Lee. Hydrothermal/solvothermal synthesis and treatment of TiO2 for photocatalytic degradation of air pollutants: Preparation, characterization, properties, and performance, Chemosphere, 219 (2019), pp. 804-825

E. Grabowska, M. Marchelek, T. Klimczuk, G. Trykowski, A. Zaleska-Medynska. Noble metal modified TiO2 microspheres: Surface properties and photocatalytic activity under UV–vis and visible light, Journal of Molecular Catalysis A: Chemical, 423 (2016), pp. 191-206

Z. Wu, Z. Gu, W. Zhao, H. Wang. Photocatalytic oxidation of gaseous benzene over nanosized TiO2 prepared by solvothermal method, Chinese Science Bulletin, 52 (2007), pp. 3061-3067

M.-V. Sofianou, C. Trapalis, V. Psycharis, N. Boukos, T. Vaimakis, J. Yu, W. Wang. Study of TiO2 anatase nano and microstructures with dominant {001} facets for NO oxidation, Environmental Science and Pollution Research, 19 (2012), pp. 3719-3726

R. Shahbazi, A. Payan, M. Fattahi. Preparation, evaluations and operating conditions optimization of nano TiO2 over graphene based materials as the photocatalyst for degradation of phenol, Journal of Photochemistry and Photobiology A: Chemistry, 364 (2018), pp. 564-576

R. Wang, X. Cai, F. Shen. Preparation of TiO2 hollow microspheres by a novel vesicle template method and their enhanced photocatalytic properties, Ceramics International, 39 (2013), pp. 9465-9470

X. Li, J. Yu, M. Jaroniec. Hierarchical photocatalysts, Chemical Society Reviews, 45 (2016), pp. 2603-2636

A. Collins, D. Carriazo, S.A. Davis, S. Mann. Spontaneous template-free assembly of ordered macroporous titania, Chemical Communications (2004), pp. 568-569

Q. Zhang, W. Wang, J. Goebl, Y. Yin. Self-templated synthesis of hollow nanostructures, Nano Today, 4 (2009), pp. 494-507

J. Yu, L. Zhang, B. Cheng, Y. Su. Hydrothermal Preparation and Photocatalytic Activity of Hierarchically Sponge-like Macro-/Mesoporous Titania, The Journal of Physical Chemistry C, 111 (2007), pp. 10582-10589

H. Zhang, J.F. Banfield. Understanding Polymorphic Phase Transformation Behavior during Growth of Nanocrystalline Aggregates: Insights from TiO2, the Journal of Physical Chemistry B, 104 (2000), pp. 3481-3487

K.-i. Ishibashi, A. Fujishima, T. Watanabe, K. Hashimoto. Detection of active oxidative species in TiO2 photocatalysis using the fluorescence technique, Electrochemistry Communications, 2 (2000), pp. 207-210

E. Jimenez-Relinque, M. Castellote. Quantification of hydroxyl radicals on cementitious materials by fluorescence spectrophotometry as a method to assess the photocatalytic activity, Cement and Concrete Research, 74 (2015), pp. 108-115

R.M. Mohamed, A.A. Ismail, M.W. Kadi, D.W. Bahnemann. A comparative study on mesoporous and commercial TiO2 photocatalysts for photodegradation of organic pollutants, Journal of Photochemistry and Photobiology A: Chemistry, 367 (2018), pp. 66-73

M. Bellardita, A. Di Paola, B. Megna, L. Palmisano. Determination of the crystallinity of TiO2 photocatalysts, Journal of Photochemistry and Photobiology A: Chemistry, 367 (2018), pp. 312-320

N.M. Kinsinger, A. Wong, D. Li, F. Villalobos, D. Kisailus. Nucleation and Crystal Growth of Nanocrystalline Anatase and Rutile Phase TiO2 from a Water-Soluble Precursor, Crystal Growth & Design, 10 (2010), pp. 5254-5261

J. Yu, J.C. Yu, W. Ho, M.K.P. Leung, B. Cheng, G. Zhang, X. Zhao. Effects of alcohol content and calcination temperature on the textural properties of bimodally mesoporous titania, Applied Catalysis A: General, 255 (2003), pp. 309-320

R.L. Penn, J.F. Banfield. Morphology development and crystal growth in nanocrystalline aggregates under hydrothermal conditions: insights from titania, Geochimica et Cosmochimica Acta, 63 (1999), pp. 1549-1557

R.K. Wahi, Y. Liu, J.C. Falkner, V.L. Colvin. Solvothermal synthesis and characterization of anatase TiO2 nanocrystals with ultrahigh surface area, Journal of Colloid and Interface Science, 302 (2006), pp. 530-536

P.-T. Hsiao, M.-D. Lu, Y.-L. Tung, H. Teng. Influence of Hydrothermal Pressure during Crystallization on the Structure and Electron-Conveying Ability of TiO2 Colloids for Dye-Sensitized Solar Cells, The Journal of Physical Chemistry C, 114 (2010), pp. 15625-15632

J. Ovenstone. Preparation of novel titania photocatalysts with high activity, Journal of Materials Science, 36 (2001), pp. 1325-1329

K. Yanagisawa, J. Ovenstone. Crystallization of Anatase from Amorphous Titania Using the Hydrothermal Technique: Effects of Starting Material and Temperature, The Journal of Physical Chemistry B, 103 (1999), pp. 7781-7787

G. Li, S. Ciston, Z.V. Saponjic, L. Chen, N.M. Dimitrijevic, T. Rajh, K.A. Gray. Synthesizing mixed-phase TiO2 nanocomposites using a hydrothermal method for photo-oxidation and photoreduction applications, Journal of Catalysis, 253 (2008), pp. 105-110

J. Yu, Y. Su, B. Cheng, M. Zhou. Effects of pH on the microstructures and photocatalytic activity of mesoporous nanocrystalline titania powders prepared via hydrothermal method, Journal of Molecular Catalysis A: Chemical, 258 (2006), pp. 104-112

J.L. Blin, A. Léonard, Z.Y. Yuan, L. Gigot, A. Vantomme, A.K. Cheetham, B.L. Su. Hierarchically Mesoporous/Macroporous Metal Oxides Templated from Polyethylene Oxide Surfactant Assemblies, Angewandte Chemie International Edition, 42 (2003), pp. 2872-2875

J.G. Yu, Y.R. Su, B. Cheng. Template‐Free Fabrication and Enhanced Photocatalytic Activity of Hierarchical Macro‐/Mesoporous Titania, Advanced Functional Materials, 17 (2007), pp. 1984-1990

A. Vantomme, A. Léonard, Z.-Y. Yuan, B.-L. Su. Self-formation of hierarchical micro-meso-macroporous structures: Generation of the new concept “Hierarchical Catalysis”, Colloids and Surfaces A: Physicochemical and Engineering Aspects, 300 (2007), pp. 70-78

G. Bartosz. Use of spectroscopic probes for detection of reactive oxygen species, Clinica Chimica Acta, 368 (2006), pp. 53-76

T. Hirakawa, Y. Nosaka. Properties of O2•- and OH• Formed in TiO2 Aqueous Suspensions by Photocatalytic Reaction and the Influence of H2O2 and Some Ions, Langmuir, 18 (2002), pp. 3247-3254

W.-K. Jo, H.-J. Kang. (Ratios: 5, 10, 50, 100, and 200) Polyaniline–TiO2 composites under visible- or UV-light irradiation for decomposition of organic vapors, Materials Chemistry and Physics, 143 (2013), pp. 247-255

C.L. Bianchi, S. Gatto, C. Pirola, A. Naldoni, A. Di Michele, G. Cerrato, V. Crocellà, V. Capucci. Photocatalytic degradation of acetone, acetaldehyde and toluene in gas-phase: Comparison between nano and micro-sized TiO2, Applied Catalysis B: Environmental, 146 (2014), pp. 123-130

H. Lin, J. Long, Q. Gu, W. Zhang, R. Ruan, Z. Li, X. Wang. In situ IR study of surface hydroxyl species of dehydrated TiO2: towards understanding pivotal surface processes of TiO2 photocatalytic oxidation of toluene, Physical Chemistry Chemical Physics, 14 (2012), pp. 9468-9474

J. Araña, J.M. Doña-Rodrı́guez, O. González-Dı́az, E. Tello RendónJ.A. Herrera Melián, G. Colón, J.A. Navı́o, J. Pérez Peña, Gas-phase ethanol photocatalytic degradation study with TiO2 doped with Fe, Pd and Cu, Journal of Molecular Catalysis A: Chemical, 215 (2004), pp. 153-160

J. Araña, A.P. Alonso, J.M.D. Rodríguez, G. Colón, J.A. Navío, J.P. Peña. FTIR study of photocatalytic degradation of 2-propanol in gas phase with different TiO2 catalysts, Applied Catalysis B: Environmental, 89 (2009), pp. 204-213

A.H. Mamaghani, F. Haghighat, C.-S. Lee. Gas phase adsorption of volatile organic compounds onto titanium dioxide photocatalysts, Chemical Engineering Journal, 337 (2018), pp. 60-73

A.H. Mamaghani, H. Fariborz, L. Chang-Seo. Photocatalytic oxidation of MEK over hierarchical TiO2 catalysts: Effect of photocatalyst features and operating conditions, Applied Catalysis B: Environmental (2019)

A. Haghighatmamaghani, F. Haghighat, C.-S. Lee. Performance of various commercial TiO2 in photocatalytic degradation of a mixture of indoor air pollutants: Effect of photocatalyst and operating parameters, Science and Technology for the Built Environment (2018), pp. 1-15

L. Zhong, F. Haghighat, C.-S. Lee, N. Lakdawala. Performance of ultraviolet photocatalytic oxidation for indoor air applications: Systematic experimental evaluation, Journal of Hazardous Materials, 261 (2013), pp. 130-138

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