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Article

Synthesis and Growth Mechanism of Titanate and Titania One-Dimensional Nanostructures Self-Assembled into Hollow Micrometer-Scale Spherical Aggregates

Supporting Info

Yuanbing Mao,^† Mandakini Kanungo,^‡ Tirandai Hemraj-Benny,^† and Stanislaus S. Wong*^†^‡

Department of Chemistry, State University of New York at Stony Brook, Stony Brook, New York 11794-3400, and Materials and Chemical Sciences Department, Brookhaven National Laboratory, Building 480, Upton, New York 11973

J. Phys. Chem. B, 2006, 110 (2), pp 702–710

DOI: 10.1021/jp0544538

Publication Date (Web): December 18, 2005

†

State University of New York at Stony Brook.

‡

Brookhaven National Laboratory.

To whom correspondence should be addressed. Tel: 631-632-1703. E-mail: sswong@notes.cc.sunysb.edu. Tel: 631-344-3178. E-mail: sswong@bnl.gov.

Abstract

Three-dimensional, dendritic micrometer-scale spheres of alkali metal hydrogen titanate 1D nanostructures (i.e., nanowires and nanotubes) have been generated using a modified hydrothermal technique in the presence of hydrogen peroxide and an alkali metal hydroxide solution. Sea-urchin-like assemblies of these 1D nanostructures have been transformed into their hydrogen titanate analogues (lepidocrocite H_xTi₂_-_x_/4□_x_/4O₄ (x 0.7, □: vacancy)) by neutralization as well as into their corresponding anatase TiO₂ nanostructured counterparts through a moderate high-temperature annealing dehydration process without destroying the 3D hierarchical structural motif. The as-prepared hollow spheres of titanate and titania 1D nanostructures have overall diameters, ranging from 0.8 to 1.2 μm, while the interior of these aggregates are vacuous with a diameter range of 100 to 200 nm. The constituent, component titanate and TiO₂ 1D nanostructures have a diameter range of 7 ± 2 nm and lengths of up to several hundred nanometers. A proposed two-stage growth mechanism of these hollow micrometer-scale spheres was supported by time-dependent scanning electron microscopy, atomic force microscopy, and inductively coupled plasma atomic emission spectrometry data. We have also demonstrated that these assemblies are active photocatalysts for the degradation of synthetic Procion Red dye under UV light illumination.