Combustion synthesis (CS) is an attractive method for producing advanced materials, including ceramics, intermetallics, and composites. In this process, after initiation by an external heat source, a highly exothermic reaction propagates through the sample in a self-sustained combustion wave. The process offers the possibility of producing materials with novel structures and properties.; At conventional magnifications and imaging rates, the combustion wave appears to propagate in a planar, steady manner. However, using higher magnifications ({dollar}>{dollar}400X) and imaging rates (1000 frames/sec), fluctuations in the shape and propagation of the combustion front were observed. These variations in local conditions (i.e., the microstructure of the combustion wave) can influence the microstructure and properties of materials produced by combustion synthesis.; In this work, the microstructure of wave propagation during combustion synthesis is investigated experimentally and theoretically. Using microscopic high-speed imaging, the spatial and temporal fluctuations of the combustion front shape and propagation were investigated. New image analysis methods were developed to characterize the heterogeneity of the combustion front quantitatively. The initial organization of the reaction medium was found to affect the heterogeneity of the combustion wave.; Moreover, at the microscopic level, two different regimes of combustion propagation were observed. In the quasihomogeneous mechanism, the microstructure of the combustion wave resembles what is viewed macroscopically, and steady, planar propagation is observed. In the relay-race mechanism, while planar at the macroscopic level, the combustion front profiles are irregularly shaped, with arc-shaped convexities and concavities at the microscopic level. Also, the reaction front propagates as a series of rapid jumps and hesitations. Based on the combustion wave microstructure, new criteria were developed to determine the boundaries between quasihomogeneous and relay-race mechanisms, as functions of the initial organization of the reaction medium (i.e. particle size and porosity).; In conjunction with the experiments, a microheterogeneous cell model was developed that simulates the local propagation of the combustion wave. Accounting for the stochastically organized medium with non-uniform properties, calculated results for the microstructural parameters of the combustion wave, and their dependence on density and reactant particle size, were in good qualitative agreement with experimental data.
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