The Compelling Case for Indentation as a Functional Exploratory and Characterization Tool

The utility of indentation testing for characterizing a wide range of mechanical properties of brittle materials is highlighted in light of recent articles questioning its validity, specifically in relation to the measurement of toughness. Contrary to assertion by some critics, indentation fracture theory is fundamentally founded in Griffith–Irwin fracture mechanics, based on model crack systems evolving within inhomogeneous but well-documented elastic and elastic–plastic contact stress fields. Notwithstanding some numerical uncertainty in associated stress intensity factor relations, the technique remains an unrivalled quick, convenient and economical means for comparative, site-specific toughness evaluation. Most importantly, indentation patterns are unique fingerprints of mechanical behavior and thereby afford a powerful functional tool for exploring the richness of material diversity. At the same time, it is cautioned that unconditional usage without due attention to the conformation of the indentation patterns can lead to overstated toughness values. Limitations of an alternative, more engineering approach to fracture evaluation, that of propagating a pre-crack through a 'standard' machined specimen, are also outlined. Misconceptions in the critical literature concerning the fundamental nature of crack equilibrium and stability within contact and other inhomogeneous stress fields are discussed.This is the author accepted manuscript. The final version is available from Wiley via http://dx.doi.org/10.1111/jace.1372

Characterization of Films with Thickness Less than 10 nm by Sensitivity-Enhanced Atomic Force Acoustic Microscopy

We present a method for characterizing ultrathin films using sensitivity-enhanced atomic force acoustic microscopy, where a concentrated-mass cantilever having a flat tip was used as a sensitive oscillator. Evaluation was aimed at 6-nm-thick and 10-nm-thick diamond-like carbon (DLC) films deposited, using different methods, on a hard disk for the effective Young's modulus defined as E/(1 - ν2), where E is the Young's modulus, and ν is the Poisson's ratio. The resonant frequency of the cantilever was affected not only by the film's elasticity but also by the substrate even at an indentation depth of about 0.6 nm. The substrate effect was removed by employing a theoretical formula on the indentation of a layered half-space, together with a hard disk without DLC coating. The moduli of the 6-nm-thick and 10-nm-thick DLC films were 392 and 345 GPa, respectively. The error analysis showed the standard deviation less than 5% in the moduli

Elastic Properties of 4–6 nm-thick Glassy Carbon Thin Films

Glassy carbon is a disordered, nanoporous form of carbon with superior thermal and chemical stability in extreme environments. Freestanding glassy carbon specimens with 4–6 nm thickness and 0.5 nm average pore size were synthesized and fabricated from polyfurfuryl alcohol precursors. Elastic properties of the specimens were measured in situ inside a scanning electron microscope using a custom-built micro-electro-mechanical system. The Young’s modulus, fracture stress and strain values were measured to be about 62 GPa, 870 MPa and 1.3%, respectively; showing strong size effects compared to a modulus value of 30 GPa at the bulk scale. This size effect is explained on the basis of the increased significance of surface elastic properties at the nanometer length-scale

Depth-resolved residual stress analysis of thin coatings by a new FIB-DIC method

"A new methodology for the measurement of depth sensitive residual stress profiles of thin coatings with sub-micrometer resolution is presented. The two step method consists of incremental focused ion beam (FIB) ring-core milling, combined with high-resolution in situ SEM-FEG imaging of the relaxing surface and a full field strain analysis by digital image correlation (DIC). The through-thickness profile of the residual stress can be obtained by comparison of the experimentally measured surface strain with finite element modeling using Schajer's integral method. In this work, a chromium nitride (CrN) CAE-PVD 3.0 mu m coating on steel substrate, and a gold MS-PVD 1.5 mu m on silicon were selected for the experimental implementation. Incremental FIB milling was conducted using an optimized milling strategy that produces minimum re-deposition over the sample surface. Results showed an average residual stress of sigma = -5.15 GPa in the CrN coating and sigma = +194 MPa in the Au coating. These values are in reasonable agreement with estimates obtained by other conventional techniques. The depth profiles revealed an increasing residual stress from surface to the coating\/surface interface for both coatings. This observation is likely related to stress relaxation during grain growth, which was observed in microstructural cross sections, as predicted by existing models for structure-stress evolution in PVD coatings. A correlation between the observed stress gradients and the in-service mechanical behavior of the coatings is proposed. Finally, critical aspects of the technique and the influence of microstructure and elastic anisotropy on stress analysis are analyzed and discussed. (C) 2011 Elsevier B.V. All rights reserved.

Discussion on "Interfacial Residual Stress Analysis of Thermal Spray Coatings by Miniature Ring-Core Cutting Combined with DIC Method" by J.G. Zhu et al., Experimental Mechanics DOI:10.1007/s11340-012-9640-2

In this article authors present similarities between an article by J.G. Zhu and colleagues regarding measurement of the residual stress in thermal barrier coatings (TBCs) using a self developed deformation sensor and the article regarding the same by M. Sebastiani and colleagues published in the previous issue. Topics discussed include similarity in experimental implementation, use of scanning electron microscope images, and use of micro-ring core method for thermal spray coatings