Calibrating a nanoindenter for very shallow depth indentation using equivalent contact radius

Nanoindenter tips are usually modelled as axisymmetric cones, with calibration involving finding a fitting function that relates contact area to contact depth. For accurate calibration of shallow depth indentation, this is not ideal because it means that deeper indents tend to dominate the fitting function. For an axisymmetric object, it is always possible to define an equivalent contact radius (which, in the case, of nanoindentation is linearly related to the reduced modulus) and to obtain a fitting function that relates this equivalent contact radius to indentation depth. The equivalent contact radius approach is used here to provide shallow depth calibration of a nanoindenter tip at three separate times. The advantage of the equivalent contact radius methodology is that it provides a clearer physical interpretation of the changes in tip shape than a conventional area-based fit. We also show that the minimum depth for a reliable hardness measurement is obtainable and increases as the tip blunts with age but that consistent measurements of very near surface elastic moduli can be made if the blunting of the tip over time is fully accounted for in the tip area function calibration.     

Compositional dependence of serrated flow in nickel binary solid solutions during high-temperature microindentation

At 450?°C, pure nickel and nickel binary solid solutions, containing Ru, Rh, W, Re, Ir and Pt, have a smooth load–depth curves. In contrast, the alloying addition of Nb, Mo, Pd and Ta results in the occurrence of serrations in their load–depth profiles. Analyses show the load increment of the quasi-elastic segments scales linearly with the load at their starting point. The slope of such linear relationships was normalized by the solute concentration and then plotted against the diffusion rate of transition metal solutes within the nickel lattice and along dislocation cores. Linear relationships were observed in both cases. Results suggest that the solute diffusion along dislocation cores coupled with the atomic size misfit are mainly responsible for such serrations.     

Hexagonal germanium formed via a pressure‐induced phase transformation of amorphous germanium under controlled nanoindentation

We have studied the stable end phase formed in amorphous germanium (a‐Ge) films that have been subjected to a pressure‐induced phase transformation under indentation loading using a large (20 µm) spherical indenter. After indentation the samples have been annealed at room temperature to remove any residual unstable R8 and BC8 phases. Raman spectroscopy indicates a single broad peak centred around 292 cm^–1 and we have used first principles density functional perturbation theory calculations and simulated Raman spectra for nano‐crystalline diamond cubic germanium (DC‐Ge) to help identification of the final phase as hexagonal diamond germanium (HEX‐Ge). Transmission electron microscopy and selected area diffraction analysis confirmed the presence of a dominant HEX‐Ge end phase. These results help explain significant inconsistencies in the literature relating to indentation‐induced phase transitions in DC‐ and a‐Ge. (© 2013 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Effect of repetition nanoindentation of GaN epilayers on a‐axis sapphire substrates

In this work, gallium nitride (GaN) epilayers were deposited on a‐axis sapphire substrate by means of metal organic chemical vapor deposition (MOCVD). Berkovich nanoindentation was used to explore the repetition pressure‐induced impairment of the GaN film. The observation of load‐displacement vs stress‐strain curves concludes that basal slip is implicated in the deformation on the A plane GaN. The increase in the hardness (H) and elastic modulus (E) was determined from cyclic nanoindentation, and resulted in a crack due to the formation of incipient slip bands and/or the to‐and‐fro motion of mobile dislocation. It is indicated that the generation of individual dislocation and residual deformation of the GaN films are showed by CL mapping analysis. From the morphological studies, it is revealed that the crack was found by means of atomic force microscope (AFM) technique at nine loading/reloading cycles even after the indentation beyond the critical depth on the residual indentation impression. Copyright © 2010 John Wiley & Sons, Ltd.     

Effect of irradiation on microstructure and hardening of Cr–Fe–Ni–Mn high-entropy alloy and its strengthened version

ABSTRACT

A single-phase fcc high-entropy alloy (HEA) of 20%Cr–40%Fe–20%Mn–20%Ni composition and its strength with yttrium and zirconium oxides version was irradiated with 1.4?MeV Ar ions at room temperature and mid-range doses from 0.1 to 10 displacements per atom (dpa). Transmission electron microscopy (TEM), scanning transmission electron microscopy with energy dispersive X-ray spectrometry (STEM/EDS) and X-ray diffraction (XRD) were used to characterise the radiation defects and microstructural changes. Nanoindentation was used to measure the ion irradiation effect on hardening. In order to understand the irradiation effects in HEAs and to demonstrate their potential advantages, a comparison was performed with hardening behaviour of 316 austenitic stainless steel irradiated under an identical condition. It was shown that hardness increases with irradiation dose for all the materials studied, but this increase is lower in high-entropy alloys than in stainless steel.     

Analytical methods to derive the elastic modulus of soft and adhesive materials from atomic force microcopy force measurements

We present new DMT‐based and JKR‐based methods to derive the elastic modulus of sample surfaces from an atomic force microscope force‐distance curve (DMT: Derjaguin‐Muller‐Toporov, JKR: Johnson–Kendall–Roberts). Application of the methods to the Maugis–Dugdale curves revealed that the JKR‐based method determines very accurate moduli for Maugis' transitional parameter λ > 0.3; however, the DMT‐based method generally estimates much less accurate moduli. The new JKR‐based method has advantages over the two‐point method, which has been often used for the JKR analysis, in capabilities to select the fitting range and to involve more than two points in curve fitting. Utilizing the advantages, for example, one can limit the fitting range to the attractive force zone to reduce the contact area of soft and adhesive materials. The method consists of algebraical calculation and optionally linear fitting; hence, the computational cost is low enough to be applicable to a real‐time JKR analysis method of fast force mapping. The detailed procedure of the method is explained using a force‐distance curve on a poly(dimethylsiloxane) surface. The advantages of the method are demonstrated using a force mapping data on a vulcanized rubber blend. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2019 , 57, 1279–1286     

Dislocation slip behaviors in high-quality bulk GaN investigated by nanoindentation

The dislocation slip behaviors in GaN bulk crystal are investigated by nanoindentation, the dislocation distribution patterns formed around an impress are observed by cathodoluminescence (CL) and cross-sectional transmission electron microscope (TEM). Dislocation loops, vacancy luminescence, and cross-slips show hexagonal symmetry around the <11-20> and <1-100> direction on c-plane. It is found that the slip planes of dislocation in GaN crystal are dominated in {0001} basal plane and {10-11} pyramid plane. According to the dislocation intersection theory, we come up with the dislocation formation process and the related mechanisms are discussed.     

Determination of elastic and plastic mechanical properties of dentin based on experimental and numerical studies

The aim of this study is to investigate the change of mechanical properties of human dentin due to aging and spatial variation. Sections of coronal dentin are made from human molars in three groups: young, mid-aged, and old patients. A nanoindentation test is conducted from regions near the pulp to the dentin-enamel junction (DEJ) to evaluate the load-depth indentation response and determine Young's modulus and hardness. Based on the loading and unloading load-displacement curves in nanoindentation, a numerical model of plastic damage is used to study the plastic and the damage behaviors and the contribution to the degradation in the unloading stiffness. The experimental results show that Young's modulus of the inner dentin is significantly lower than that of outer dentin in each age group. Compared with the young dentin, the old dentin has greater hardness and Young's modulus with similar spatial variations. The magnitudes of the yield strength and the damage variable are also affected by aging and vary with spatial locations. In the same age group, the yield strength in inner dentin is lower than those in middle and outer dentin, more damage occurs with similar spatial variations, and the yield strength of young dentin is generally lower and causes more damage compared with those in both the mid-aged and old groups.     

Dislocation-mediated creep process in nanocrystalline Cu

Nanocrystalline Cu with average grain sizes ranging from ～ 24.4 to 131.3 nm were prepared by the electric brushplating technique.Nanoindentation tests were performed within a wide strain rate range,and the creep process of nanocrystalline Cu during the holding period and its relationship to dislocation and twin structures were examined.It was demonstrated that creep strain and creep strain rate are considerably significant for smaller grain sizes and higher loading strain rates,and are far higher than those predicted by the models of Cobble creep and grain boundary sliding.The analysis based on the calculations and experiments reveals that the significant creep deformation arises from the rapid absorption of high density dislocations stored in the loading regime.Our experiments imply that stored dislocations during loading are highly unstable and dislocation activity can proceed and lead to significant post-loading plasticity.     

Molecular dynamics study of plastic deformation mechanism in Cu/Ag multilayers

The plastic deformation mechanism of Cu/Ag multilayers is investigated by molecular dynamics(MD) simulation in a nanoindentation process. The result shows that due to the interface barrier, the dislocations pile-up at the interface and then the plastic deformation of the Ag matrix occurs due to the nucleation and emission of dislocations from the interface and the dislocation propagation through the interface. In addition, it is found that the incipient plastic deformation of Cu/Ag multilayers is postponed, compared with that of bulk single-crystal Cu. The plastic deformation of Cu/Ag multilayers is affected by the lattice mismatch more than by the difference in stacking fault energy(SFE) between Cu and Ag. The dislocation pile-up at the interface is determined by the obstruction of the mismatch dislocation network and the attraction of the image force. Furthermore, this work provides a basis for further understanding and tailoring metal multilayers with good mechanical properties, which may facilitate the design and development of multilayer materials with low cost production strategies.