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SiO 2 -TiO 2 composite nanoparticle assemblies with or without alkyl surface modification and bearing a higher-order hollow spherical morphology were successfully synthesized by a simple, rapid, one-pot, and single-step solvothermal method using a precursor solution consisting of n-octyl-Si(OMe) 3 or Si(OEt) 4 , Ti(OiPr) 4 , o-phthalic acid, and acetic acid in methanol. The addition of acetic acid is essential for a high yield of nanoparticle assemblies with hollow spherical morphology and a high content of Si. The Si/Ti atomic ratio in the SiO 2 -TiO 2 com-

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