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In Part III of this series, experimental optimization of the laser spallation technique is achieved by investigating the effect of the kind and thickness of the constraining materials and the energy‐absorbing film on the amplitude and profile of the generated stress pulse. An experimental setup consisting of a 0.5‐μm‐thick Al film as the energy absorbing film and a 5 μm layer of solid water glass as the constraining material is found to maximize the stress pulse amplitude. In addition, the effect of the substrate material on the shape of the stress pulse is also determined. Finally, it was found that for a given substrate, the pulse profile is independent of the laser fluence, indicating similar laser‐material interaction phenomena over the range of fluence levels considered here.