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Materials whose dielectric constant varies spatially with submicrometer periodicity exhibit diffractive optical properties which are potentially valuable in a number of existing and emerging applications. Here, such systems are fabricated by exploiting the spontaneous crystallization of monodisperse silica spheres into close-packed arrays. By reliance on a vertical deposition technique to pack the spherical colloids into close-packed silica−air arrays, high quality samples can be prepared with thicknesses up to 50 μm. These samples are planar and thus suitable for optical characterization. Scanning electron microscopy (SEM) of these materials illustrates the close-packed ordering of the spherical colloids in planes parallel to the substrate; cross-sectional SEM micrographs of the arrays as well as optical methods are used to measure sample thickness and uniformity. Normal-incidence transmission spectra in the visible and near-infrared regions show distinct peaks due to diffraction from the colloidal layers. While these basic optical characteristics are similar to thicker and polycrystalline gravity-sedimented colloidal crystals, the systematic control over the number of colloidal layers allows the effect of sample thickness on the optical spectrum to be studied for the first time.