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10. Effects of layer thickness on the mechanical behavior of oxidation-strengthened Zr/Nb nanoscale multilayers

Author

Monclús, M. A., Callisti, M., Polcar, T., Yang, L. W., Molina-Aldareguía, J. M., and LLorca, J.

Subjects
Condensed Matter - Materials Science
Abstract

The mechanical behaviour and deformation mechanisms of magnetron-sputtered Zr/Nb nanoscale multilayers were analysed as a function of the periodicity (L = 10 and 75 nm) and annealing time at 350C (2-336 hrs). The strength of the as-deposited multilayers was independent of the layer thickness and it was controlled by the co-deformation of the Zr and Nb layers. Annealing led to transformation of the Zr layers into ZrO2 after a few hours, while the Nb layers oxidised at a much slower rate. The volumetric expansion associated with the oxidation led to the formation of cracks at the interfaces and within the ZrO2 layers for the multilayers with L = 75 nm but not in the case of L = 10 nm. The nanoindentation hardness increased significantly after annealing due to the contribution of the residual stresses associated with the volume increase due to oxidation and to the higher strength of the oxides. The strength increase after annealing, as measured by micropillar compression tests, was smaller than that measured by nanoindentation, as it did not include the contribution of the residual stresses, which were relieved during micropillar fabrication. The nanolaminate with L = 10 nm presented the highest strength and toughness as damage during oxidation was suppressed, and a deformation mechanism controlled by the formation of shear bands.

Published
2017
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12. Selective oxidation-induced strengthening of Zr/Nb nanoscale multilayers

Author

Monclús, M. A., Callisti, M., Polcar, T., Yang, L. W., LLorca, J., and Molina-Aldareguía, J. M.

Subjects
Condensed Matter - Materials Science
Abstract

The paper presents a new approach, based on controlled oxidation of nanoscale metallic multilayers, to produce strong and hard oxide/metal nanocomposite coatings with high strength and good thermal stability. The approach is demonstrated by performing long term annealing on sputtered Zr/Nb nanoscale metallic multilayers and investigating the evolution of their microstructure and mechanical properties by combining analytical transmission electron microscopy, nano-mechanical tests and finite element models. As-deposited multilayers were annealed at 350 C in air for times ranging between 1 - 336 hours. The elastic modulus increased by approx. 20% and the hardness by approx. 42% after 15 hours of annealing. Longer annealing times did not lead to changes in hardness, although the elastic modulus increased up to 35% after 336 hrs. The hcp Zr layers were rapidly transformed into monoclinic ZrO2 (in the first 15 hours), while the Nb layers were progressively oxidised, from top surface down towards the substrate, to form an amorphous oxide phase at a much lower rate. The sequential oxidation of Zr and Nb layers was key for the oxidation to take place without rupture of the multi-layered structure and without coating spallation, as the plastic deformation of the metallic Nb layers allowed for the partial relieve of the residual stresses developed as a result of the volumetric expansion of the Zr layers upon oxidation. Moreover, the development of residual stresses induced further changes in mechanical properties in relation to the annealing time, as revealed by finite element simulations.

Published
2016
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