Attempts to prepare macroporous silica particles and metal-compound-nanoparticle-embedded silica microspheres were carried out using reactions between silicon tetrachloride and ultrasonic generating microdroplets including metal (Na, K, Al, Ni Ti, Pt) compounds. Samples were collected by dry and wet processes. In the case of using nickel and aluminum compounds, acid-treated samples were also prepared. The obtained samples were characterized by scanning electron microscopy, X-ray fluorescence spectroscopy, powder X-ray diffractometry, mercury porosimetry, and the nitrogen adsorption method. The macroporous silica particles were prepared by removing the salt crystals, such as NaCl and KCl, formed in the silica frame. For acid-resistant metals, platinum- and titanium-compound nanoparticles are easily embedded in silica microspheres using these metal-compound solutions. For acid-soluble metals, aluminum- and nickel-compound-nanoparticle-embedded silicas were prepared by applying neutralization of the collection water. Micropores and mesopores were produced in wet-process samples. Acid treatment induced the increase of micropore volumes. (c) 2005 Elsevier Inc. All rights reserved.