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The use of steady-state and time-resolved fluorescence spectroscopy to probe the internal microenvironment of sol−gel-derived organic−inorganic nanocomposites formed from alkoxysilane precursors is reviewed. The review focuses on the use of small organic probes and fluorescent biomolecules that provide information on pore−solvent composition and polarity, internal solvent and dopant dynamics, environmental heterogeneity and phase segregation, and surface chemistry, as determined by molecule−matrix interactions. Emphasis is placed on advanced fluorescence methods that can provide unique information on sol−gel-derived composite materials. The discussion begins with a description of the different fluorescent probes that have been used to study sol−gel materials. The application of fluorescence methods to examine Class I and Class II hybrid materials is then described, highlighting the specific …