Artificial multilayers, or microlaminates, composed of alternating layers of Nb and MoSi2 of equal thickness were synthesized by d.c., magnetron sputtering. Four different modulation wavelengths, λ, were studied: 7, 11, 20, and 100 nm. The compositions, periodicities, and microstructures of the microlaminates were characterized by Auger electron spectroscopy and transmission electron microscopy. Structural characterization revealed that the as-deposited Nb layers are polycrystalline, while the MoSi2 layers are amorphous. The hardnesses and elastic moduli of the films were measured using nanoindentation techniques. Neither a supermodulus nor a superhardness effect could be identified in the range of wavelengths investigated; for each of the microlaminates, both the hardness and modulus were found to fall between the bounds set by the properties of the monolithic Nb and MoSi2 films. Nevertheless, a modest but a measurable increase in both hardness and modulus with decreasing wavelength was observed, thus indicating that behavior cannot be entirely described by a simple rule-of-mixtures. The hardness was found to vary linearly with Δ−1/2 in a manner similar to the Hall–Petch relationship. Annealing the microlaminates at 800 °C for 90 min produces significant increases in hardness and modulus due to chemical interaction of the layers.