Surfactant‐Free Solvothermal Method for Synthesis of Mesoporous Nanocrystalline TiO2 Microspheres with Tailored Pore Size

Yajing Zhang,Sujuan Zhang,Jing Wu,Fu Ding,Kangjun Wang

doi:10.1155/2013/294020

Yajing Zhang, Sujuan Zhang + Show 3 more

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https://doi.org/10.1155/2013/294020

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Abstract

TiO2 mesoporous microspheres self‐assembled from nanoparticles were synthesized by a surfactant‐free solvothermal route. The TiO2 precursors were fabricated by tetrabutyl titanate, glacial acetic acid, and urea in the ethanol solution at 140°C for 20 h, and TiO2 mesoporous microspheres were obtained by a postcalcination at temperatures of 450°C for promoting TiO2 crystallization and the removal of residual organics. The phase structure, morphology, and pore nature were characterized by XRD, SEM, and nitrogen adsorption‐desorption measurements. The as‐prepared TiO2 microspheres are in anatase phase, with 2‐3 μm in diameter, and narrow pore distribution range is 3‐4 nm. The adjustments of the synthetic parameters lead to the formation of the mesoporous TiO2 microspheres with tuned pore size distributions and morphology.

Highlights

The existence of a close relationship between specific morphologies and unique properties in nanomaterials has ignited much attention to the synthesis of novel nanostructures for a broad domain of applications in the past decade [1]
Hydrothermal method has been widely used for preparing mesoporous TiO2 owing to the controllable morphology and porous structure as well as the high crystallization degree of the product [9]
The rutile phase is more stable than the anatase phase

Summary

Introduction

The existence of a close relationship between specific morphologies and unique properties in nanomaterials has ignited much attention to the synthesis of novel nanostructures for a broad domain of applications in the past decade [1]. After synthesis, the template has to be removed from the sample to make the pores accessible This can be achieved by thermal treatment (calcination) or solvents extraction [16]. TiO2 mesoporous materials are calcined; the thermal treatment processes frequently lead to the partial or total collapse of the porous structure during the template removal process and result in the decrease of the surface area [17]. The diameters size, pore volume, BET surface areas, and the pore size distributions can be tuned by adjusting synthesis parameters. This synthesis method can be extended for the fabrication of other mesoporous metal oxide materials

Experimental Section

Results and Discussion

Conclusions