Growth of single-crystal TiN/VN strained-layer superlattices with extremely high mechanical hardness

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Abstract
Single‐crystal TiN/VN strained‐layer superlattices (SLS’s) with layer thicknesses lTiN =lVN =λ/2 (where λ is the period of the superlattice) ranging from 0.75 to 16 nm have been grown on MgO(100 ) substrates by reactive magnetron sputtering. Cross‐sectional transmission electron microscopy (TEM) and x‐ray diffraction examinations showed that the films were single crystals exhibiting coherent interfaces and several orders of superlattice reflections. There was no evidence in either plan‐view or cross‐sectional TEM analyses of misfit interfacial dislocation arrays. The primary defects observed were dislocation loops with a diameter of 8–10 nm extending through several layers and small defects with a diameter of 1–2 nm that were confined within single layers. Microindentation hardness values H, measured as a function of λ in films with a total thickness of 2.5 μm, increased from 2035±280 kg mm−2 for Ti0.5V0.5N alloys (i.e., λ=0) to reach a maximum of 5560±1000 kg mm−2 at λ=5.2 nm and then decreased rapidly to 3950±550 kg mm−2 at λ=7.5 nm. Further increases in λ resulted in a slower decrease in H to 3640±550 kg mm−2 at λ=32 nm. The large error bars in the H values for the SLS samples were due to the difficulty in measuring such extremely high hardnesses in thin films. (H for pure single‐crystal TiN and VN films were 2200±300 and 1620±200 kg mm−2, respectively.) SLS samples grown with constant λ=6.5 nm, but different lTiN /λ ratios, exhibited a maximum hardness at lTiN /λ≂0.3.