Sv. Hainsworth et Tf. Page, NANOINDENTATION STUDIES OF CHEMOMECHANICAL EFFECTS IN THIN-FILM COATED SYSTEMS, Surface & coatings technology, 68, 1994, pp. 571-575
Recently, nanoindentation techniques have been successfully used to st
udy chemomechanical effects on the very near-surface mechanical proper
ties of single-crystal sapphire. In order to investigate whether such
chemomechanical effects also occur in ceramic-coated systems, a series
of experiments have been performed on a 100 nm TiN coating (over a 10
0 nm Ti interlayer) on a silicon substrate. Indentation loads were cho
sen to produce displacements less than and greater than the coating th
ickness. The specimens were annealed at low temperature in a vacuum ov
en for 24 h to desorb any physi- or chemisorbed surface species and th
en exposed to several environments including water and a series of alc
ohols and tested dry. Three distinct effects were observed. At displac
ements greater than the coating thickness, some environments (especial
ly water) produce fracture of the coating around indentations although
no differences in the load-displacement responses of the different en
vironments were evident. At very low loads (1 mN) some evidence was fo
und for both dislocation nucleation and plasticity being environmental
ly sensitive with ethanol and methanol extending the load range over w
hich ''elastic-only'' response occurs on surface contact. Further, all
low load results displayed pronounced irreproducibility and ''wavines
s'' at a spatial scale commensurate with the microstructure suggesting
that even the low temperature anneal had relaxed the stresses providi
ng structural cohesion and allowed ready ingress of liquids etc.