This article reports findings when using a molybdenum–tungsten (MoW) interlayer for diamond thin film deposition on steel substrates. The main focus was on the postdeposition stress within the diamond films and its impact on the coating's tribological properties. The effect of MoW interlayer thickness and the effect of chemical vapor deposition (CVD) process temperature have been investigated. Nanocrystalline diamond films were deposited on steel substrates with MoW interlayers (thickness of 1.1, 4.5, and 8.3 μm) at two different deposition temperatures (650 and 875 °C). It was found that when depositing good quality diamond films on steel substrates, increasing interlayer thickness and decreasing CVD process temperature have to be jointly considered to obtain the optimal result. The diamond-coated steel substrates with the 8.3 μm interlayer deposited at the lower CVD processing temperature exhibited the least residual stress combined with excellent mechanical properties.

A modeling method to extract the mechanical properties of ultra-thin films (10–100 nm thick) from experimental data generated by indentation of freestanding circular films using a spherical indenter is presented. The relationship between the mechanical properties of the film and experimental parameters including load, and deflection are discussed in the context of a constitutive material model, test variables, and analytical approaches. Elastic and plastic regimes are identified by comparison of finite element simulation and experimental data.

This paper proposes a method for determining the mechanical properties (Young's modulus, Poisson's ratio, yield strength, and work hardening factor) of a material at a specific point using an indentation technique that utilizes a specially designed indenter in conjunction with an inverse problem and finite element analyses. The specially designed indenter combines the characteristics of spherical and conical indenters and can be used to produce multiple indentations at a single point. The feasibility of the proposed method for determining the local mechanical properties of a material was confirmed by detailed precision verifications in the ideal case and the worst case.

Vickers microindentation and Berkovich nanoindentation tests were carried out on a polycrystalline nickel (Ni) bulk specimen. Electron channeling contrast imaging (ECCI) in conjunction with electron backscattered diffraction was used to image and characterize plastic deformation inside and around the indents using a field emission scanning electron microscope. The ECCI was performed with a 5 keV beam energy and 0° tilt specimen position. The strain field distribution, slip lines, and Taylor lattices were imaged on an indented surface. Orientation mapping was used to investigate the local crystallographic misorientation and identify specific ⟨110⟩ slip systems. An ion milling surface preparation technique was used to remove materials from the surface which permitted the study of deformed microstructure below the indent. A dislocation density of 1011 cm−2 was calculated based on the curvature of bend contours observed in the ECCI micrographs obtained from the Vickers indents. A yield strength of 500 MPa was calculated based on the size of the strain field measured from the ECCI micrographs of the nanoindents. The combination of ion milling, ECCI, and electron backscattered diffraction was shown to be beneficial to investigate the indentation-induced plastic deformation in a polycrystalline Ni bulk specimen.

ZK60 (Mg–Zn–Zr) alloys exhibited a variation in precipitates with aging, and their mechanical properties also changed. Microindentation tests were carried out on two types of ZK60 alloys of solid solution (T4) and peak aging (T6). Microstructure and texture evolution during indentation was investigated using electron backscatter diffraction. Twinning occurred near the indentation marks in most grains. It was found that tensile twinning was dominant, and two twin variants were usually observed. Texture and microstructure evolution by twinning and slip activation was further examined by uniaxial compression test with strain. The initial random orientation gradually changed into basal fibers with strain. Some grains with nonbasal orientations aligned with the loading direction easily underwent twinning followed by slip deformation. Other grains near basal orientations revealed only slip deformation.

les différentes méthodes qui utilisent l’essai d’indentation pour estimer la ténacité sont revues et commentées. Pour les matériaux fragiles, les formules sont principalement basées sur la mesure des fissures formées par l’indenteur ou, si l’essai est instrumenté, sur les décrochements (pop-in) observés sur la courbe charge-déplacement. D’autres méthodes moins connues peuvent utiliser la mesure de l’ouverture en fond de fissure, une équivalence entre la longueur de fissure formée et l’accroissement de pénétration de l’indenteur ou le clivage provoqué par une indentation proche du bord du matériau étudié. Pour les matériaux ductiles aucune fissure n’est visible à la surface, même pour les fortes charges appliquées. Dans ce cas la ténacité est reliée par la mécanique continue du dommage à un dommage critique mis en évidence par la diminution du module d’élasticité avec l’augmentation de la profondeur d’indentation. Toutes ces méthodes permettent de calculer la ténacité avec une incertitude pouvant aller au maximum à 50 %.

In this research, we performed experimental investigations of the influence of copper presence on hardness of arsenic triselenide (As2Se3)–arsenic triiodide (AsI3) pseudobinary glasses. The samples belong to the group of chalcogenide glasses, that, when compared with oxide glasses, can be synthesized much more easily in a wide variety of compositions, allowing also fine-tuning of their properties. Here, presence of iodine (I) facilitates glass formation, whereas addition of copper (Cu) creates possibility for interesting optoelectronic properties. As it is important to study mechanical properties of materials with respect to their fabrication and manipulation, we report results of instrumented indentation testing (IIT) of bulk samples of Cux[(As2Se3)0.9(AsI3)0.1]100−x with x = 5, 10, 20, and 25 at.% of Cu. This technique enables fast determination of indentation hardness, hardness value according to Vickers and indentation modulus directly from the indentation load–displacement curves. It was shown that all these parameters increase linearly with the increase of copper content. Improvement of the mechanical properties justifies the addition of Cu into the glass matrix.

The effects of temperature and alloying elements on deformation in the high-strain-rate regime were investigated by testing fine-grained magnesium alloys with an average grain size of 2 ∼ 3 μm by a nanoindentation technique. The dynamic hardness measurements aligned well with existing quasistatic data, together spanning a wide range of strain rates, 10−3 ∼ 150/s. The high-rate hardness was influenced by various alloying elements (Al, Li, Y and Zn) to different degrees, consistent with expectations based on solid solution strengthening. Transmission electron microscopy observations of the indented region revealed no evidence for deformation twins for any alloying elements, despite the high strain-rate. The activation energy for deformation in the present alloys was found to be 85 ∼ 300 kJ/mol within the temperature range of 298 ∼ 373 K, corresponding to a dominant deformation mechanism of dislocation glide.

The work of indentation is investigated experimentally in this article. A method of using the elastic energy to extract the elastic modulus is proposed and verified. Two types of hardness related to the work of indentation are defined and examined: Hwtis defined as the total work required creating a unit volume of contact deformationand Hwp is defined as the plastic work required creating a unit volume of plastic deformation; experiments show that both hardness definitions are good choices for characterizing hardness. Several features that may provide significant insights in understanding indentation measurements are studied. These features mainly concern some scaling relationships in indentation measurements and the indentation size effects.

The effectiveness of Oliver & Pharr's (O&P's) method, Cheng & Cheng's (C&C’s) method, and a new method developed by our group for estimating Young's modulus and hardness based on instrumented indentation was evaluated for the case of yield stress to reduced Young's modulus ratio (σy/Er) ≥ 4.55 × 10−4 and hardening coefficient (n) ≤ 0.45. Dimensional theorem and finite element simulations were applied to produce reference results for this purpose. Both O&P's and C&C's methods overestimated the Young's modulus under some conditions, whereas the error can be controlled within ±16% if the formulation was modified with appropriate correction functions. Similar modification was not introduced to our method for determining Young's modulus, while the maximum error of results was around ±13%. The errors of hardness values obtained from all the three methods could be even larger and were irreducible with any correction scheme. It is therefore suggested that when hardness values of different materials are concerned, relative comparison of the data obtained from a single standard measurement technique would be more practically useful. It is noted that the ranges of error derived from the analysis could be different if different ranges of material parameters σy/Er and n are considered.

Based on a comparison of relationships between energy dissipated during indentation and the ratio of hardness to reduced elastic modulus, Malzbender has recently proposed a procedure to determine both hardness and elastic modulus from a single loading–unloading indentation curve. However, a more accurate analysis of this relationship shows that, in fact, it suffers from the same limitations as the well-known Oliver and Pharr's method; i.e., in general, the true projected imprint area has to be measured in addition to the load–penetration curve or at least two such curves obtained with different indenter geometries are to be used to unequivocally determine the hardness and the elastic modulus of a material.

In this work, we analyzed the theoretical errors of reduced Young's modulus and hardness of materials provided by single sharp indenter algorithms. According to the analysis, two conclusions can be drawn. First, various methods that use only the indentation loading and unloading curves from a single sharp indenter and omit the effect of the strain hardening exponent own the same widths of the theoretical error bands defined here. They are WEb for reduced Young's modulus and WHb for hardness. Second, the upper-bounds, BUE and BUH, and lower-bounds, BLE and BLH, of theoretical errors of the measured reduced Young's modulus and hardness might be different for different methods. These conclusions, on the one hand, are relevant to the evaluation of various established single sharp indenter algorithms. On the other hand, they provide useful information (i.e., to optimize the theoretical error bounds) for correcting an established method and the development of new single sharp indenter algorithms. According to the conclusions, an energy-based method has been devised to determine reduced Young's modulus and hardness of materials from nanoindentation tests using a standard Berkovich or Vickers indenter (equivalent to a 70.3° cone). It has been shown that the present method owns the reasonable theoretical error bounds and can provide stable results in the presence of data errors.

Instrumented indentation is often used in the study of small-scale mechanical behavior of “soft” matters that exhibit viscoelastic behavior. A number of techniques have recently been proposed to obtain the viscoelastic properties from indentation load–displacement curves. In this study, we examine the relationships between initial unloading slope, contact depth, and the instantaneous elastic modulus for instrumented indentation in linear viscoelastic solids using either conical or spherical indenters. In particular, we study the effects of “hold-at-the-peak-load” and “hold-at-the-maximum-displacement” on initial unloading slopes and contact depths. We then discuss the applicability of the Oliver–Pharr method (Refs. 29, 30) for determining contact depth that was originally proposed for indentation in elastic and elastic-plastic solids and recently modified by Ngan et al. (Refs. 20–23) for viscoelastic solids. The results of this study should help facilitate the analysis of instrumented indentation measurements in linear viscoelastic solids.

Indentation analysis based on the concept of representative strain offers an effective way of obtaining mechanical properties, especially work-hardening behavior of metals, from reverse analysis of indentation load–displacement data, and does not require measuring of the projected contact area. The definition of representative strain adopted in previous studies [e.g., Dao et al., Acta Mater.49, 3899 (2001)] has a weak physical basis, and it works only for a limited range in some sense of engineering materials. A new indentation stress-state based formulation of representation is proposed in this study, which is defined as the plastic strain during equi-biaxial loading. Extensive numerical analysis based on the finite element method has shown that with the new formulation of representative strain and representative stress, the critical normalized relationship between load and material parameters is essentially independent of the work-hardening exponent for all engineering materials, and the results also hold for three distinct indenter angles. The new technique is used for four materials with mechanical properties outside the applicable regime of previous studies, and the reverse analysis has validated the present analysis. The new formulation based on indentation stress-state based definition of representative strain has the potential to quickly and effectively measure the mechanical properties of essentially all engineering materials as long as their constitutive behavior can be approximated into a power-law form.

The high-temperature indentation fracture and microstructures of dysprosium niobate (DyNbO4) were investigated by optical, scanning, and transmission electron microscopy (OM, SEM, and TEM). Polycrystalline samples were sintered at 1350 °C for 3 h and cut into 3 mm disks for TEM. The disks were indented in a Nikon QM (Tokyo, Japan) hot hardness indenter at room temperature up to 1000 °C. Many lamellar twins having different widths were observed by TEM as well as intergranular microcracks. The room temperature hardness was relatively low at 5.64 GPa and decreased with elevated temperatures. Crack lengths were short, showing a typical micro-cracking effect. In the sample indented at 1000 °C, dislocations in periodic arrays were evident, and their density increased markedly due to heavy plastic deformation.

The critical parameters for the structural stability of physical vapor deposited TiN film on (1120) sapphire were investigated by analyzing the adhesion strength and failure mechanism through in situ observations of the fracture sequence during scratch tests and static normal indentation. TiN was deposited by arc ion plating on (1120) sapphire, and the thickness of the TiN film was controlled to 700 nm. Delamination of TiN film was monitored in situ from below the contact through a transparent sapphire substrate, using zoom optics mounted into a video imaging sensor. In situ observation enables us to detect the failure origin of TiN coating on sapphire. The failure origin of TiN film on (1120) sapphire was identified as both rhombohedral and basal twinning of the sapphire substrate. Rhombohedral twinning was initiated first, and basal twinning ensued. Twinning-induced plastic deformation of the sapphire substrate triggered the initiation of interfacial delamination of the TiN coating. The plastic deformation of the substrate ultimately induced failure of the protective coating.

Based on a comparison of relationships between the energy dissipated during indentation and the ratio of hardness to elastic modulus, a procedure is outlined to determine hardness and elastic modulus from the ratio of the elastic to total energy dissipated during an indentation cycle for non-ideal indenters.