The thermal expansion coefficient (CTE) is a vital design parameter for reducing the thermal-stress-induced structural failure of electronic chips/devices. At the micro- and nano-scale, the typical size range of the components in chips/devices, the CTEs are probably different from that of the bulk materials, but an easy and accurate measurement method is still lacking. In this paper, we present a simple but effective method for determining linear CTEs of micro-scale materials only using the prevalent nanoindentation system equipped with a heating stage for precise temperature control. By holding a constant force on the sample surface, while heating the sample at a constant rate, we measure two height–temperature curves at two positions, respectively, which are close to each other but at different heights. The linear CTE is obtained by analyzing the difference of height change during heating. This method can be applied to study the size effect or surface effect of CTE of embedded micro-scale structures, aiding the failure analysis and structural design in the semiconductor industry.

Mechanical properties of hydrogels are of considerable interest for applications including tissue engineering and drug delivery. However, mechanical characterization of hydrogels is inherently challenging due to their multiphasic construction. Under mechanical loading, internal fluid redistribution affects the gel response, leading to a time- and length-scale-dependent material behavior, known as poroelasticity. Traditional mechanical tests are effective for determining instantaneous flow-independent gel response, and they are limited in characterizing poroelastic behavior as a function of loading time- and length-scales. Here, micro- and nanoindentation experiments are combined to characterize the full range of poroelastic behavior of a hydrogel. A master curve is presented to demonstrate that the relative competition of poroelastic relaxation time with ramp loading time determines gel response across different time- and length-scales. The master curve provides a novel mechanism to establish the instantaneous and equilibrium limits on the elastic modulus for a material, useful for designing hydrogel biomaterials.

Meteorites have one of the most unique and beautiful microstructures, the Widmanstätten structure. This consists of large, elongated bands which form an intricate octahedral lace of crystalline metal. This structure makes meteorites an ideal case to demonstrate the capabilities of mechanical phase mapping using high-speed nanoindentation. In this work, the mechanical properties and composition of the Taza meteorite were mapped using ~100,000 indentations to statistically determine the properties of the individual phases. Five microstructural phases were characterized in this meteorite: Kamacite, Plessite, Tetrataenite, Cloudy Zone, and Schreibersite. Mechanical phase identification was confirmed using EDX measurements, and the first direct, point-to-point correlation of EDX and large-scale indentation maps was achieved. Mechanical phase maps showed superior phase contrast to EDX in two phases. An indentation property map or a mechanical phase map using a 2D histogram was used to visualize and statistically characterize the phases and identify trends in their relationships.

The role of negative substrate bias voltage in influencing the microstructural evolution, along with the mechanical and scratch behavior of magnetron sputtered Ni–Zr alloyed thin films, has been investigated. The films have been deposited on a Si(100) substrate by direct current (DC) magnetron co-sputtering of high-purity elemental Ni and Zr targets, using an optimized target power in an argon atmosphere at room temperature by altering the negative substrate bias voltage (0 to −80 V). The increase in negative substrate bias voltages leads to an increase in Zr content of the investigated films. The characterization techniques such as grazing incidence X-ray diffraction and high-resolution transmission electron microscopy studies confirm that an increase in the negative substrate bias voltage leads to an increase in the volume fractions of amorphous phase and Ni3Zr, but a decrease in the deposition rate, surface roughness, and average grain sizes. Hardness and Young's modulus obtained by nanoindentation, along with the coefficient of friction obtained from nano-scratch experiments, appear to be related to the relative volume fractions of both nanocrystalline and the amorphous phase. Furthermore, increase in Ni3Zr volume fraction with decrease in grain size within the crystalline part of the film, with increase in substrate bias used during deposition may have contributed to both increase in both hardness and scratch resistance.

The mechanical characterization of rocks is important in engineering design and analysis of rock-related structures. In the current researches, rocks are classified as heterogeneous materials with anisotropic behavior, and advanced methods such as combined experimental-numerical approach are developed to characterize the behavior of rocks. In this study, the nanoindentation experiment in conjunction with the generalized means method is used to determine the Young’s modulus and hardness of eight different polycrystalline granite rocks. In the first step, the Young’s modulus and hardness of granites’ constituents are determined through nanoindentation tests on pure granite minerals. Then, the properties of granites are determined using generalized means method by considering the mechanical properties of minerals, their volume fractions and an empirical constant called the microstructural coefficient. Accurate results with less than 3% error are obtained for 62.5% of the granite samples. The generalized means is introduced as a simple and effective method to characterize the mechanical properties of heterogeneous polycrystalline rocks.

Key features and applications of a unique atomic force microscope (AFM), the LiteScope™, which can be integrated into a scanning electron microscope (SEM) is reported. Using the AFM-in-SEM as one tool combines the capabilities of both systems in a very efficient way. The LiteScope design features advanced Correlative Probe and Electron Microscopy (CPEM)™ imaging technology that allows simultaneous acquisition of multiple AFM and SEM signals and their precise in-time correlation into a 3D CPEM view. AFM-in-SEM advantages are presented using several examples of applications and AFM measurement modes including CPEM, material electrical and mechanical properties together with nanoindentation, and focused ion beam (FIB) applications.

Silicon carbide (SiC) is ideally suitable as a sensor material in harsh environments. Despite the brittleness in the macroscopic scale, plasticity in SiC is observed at small component length-scales. Previous nanoindentation based study combining experiment and numerical approaches of single-crystal 6H-SiC has shown that slip activation is rather complex, and that non-basal slip could potentially dominate the plastic deformation behaviour. In this study, we investigated the local deformation response evolution of shear strain directly under and in the vicinity of the indenter tip. The results show the pyramidal slip families contribute significantly to the deformation process.

With the ever-increasing importance of nanoscale deformation phenomena in contemporary technologies, basic understanding of material behavior at the nanoscale has become of critical importance. Especially, nanomechanical testing that provides the capability to study fundamental nanoscale deformation and phase change phenomena in real time and under controlled loading conditions is essential for nanomaterial research. In this study, acoustic emission (AE) was used in situ to characterize nanoindentation-induced deformation, microfracture, and phase transformation processes intrinsic of bulk single-crystal MgO and polycrystalline Al, thin films of polycrystalline SiC, and thick films of austenitic TiNi shape-memory alloy. Scale-dependent plastic deformation and microfracture affected by the indenter tip radius and the applied normal load are interpreted in terms of the type and intensity of AE events revealed by abrupt displacement excursions in the loading response of the indented materials. The amplitudes of AE waveforms are used to examine characteristic deformation, microfracture, and phase change mechanisms in the time domain. Fast Fourier transformation and short-time Fourier transformation analyses provide further insight into the material behavior and structural changes due to indentation loading in the frequency and time-frequency domain, respectively. The methodology developed in this study represents an effective approach for nanomechanical testing and in situ characterization of nanoscale deformation, microfracture, and phase transformation phenomena.

Regarding the effect of composition on the mechanical properties of intermetallic phases such as Laves phases, there is conflicting information in the literature. Some authors observed defect hardening when deviating from stoichiometric Laves phase composition, whereas others find defect softening. Here, we present a systematic investigation of the defect state, hardness, and elastic modulus of cubic and hexagonal NbCo2 Laves phases as a function of crystal structure and composition. For this purpose, diffusion couples were prepared which exhibit diffusion layers of the cubic C15 and hexagonal C14 and C36 NbCo2 Laves phases, with concentration gradients covering their entire homogeneity ranges from 24 to 37 at.% Nb. Direct observations of dislocations and stacking faults in the diffusion layers as a function of composition were performed by electron channeling contrast imaging, and the hardness and elastic modulus were probed in the diffusion layers along the concentration gradients by nanoindentation.

Pop-in during indentation testing is a term used to indicate the sudden displacement burst during loading. Experimental data are measured during an indentation pop-in event, using displacement sensors with 20 μs time constant at 100 kHz data acquisition rate. The load–depth response during the pop-in event that occurs within 160 μs is determined after accounting for the instruments' dynamic response. Unlike the response reported in the literature for force-controlled tests, wherein the load on the sample remains constant during the pop-in, a steep load drop is observed after the onset of pop-in, followed by a significant increase in the load well beyond the load at the onset of pop-in. A model for the material and instrument's dynamic response is presented that agrees well with the experimental observations. The implications of these findings for determination of pop-in length or velocity and for performing displacement-controlled testing involving closed loop control are discussed.

Constant strain rate nanoindentation hardness measurements at high sustained strain rates cannot be made in conventional nanoindentation testing systems using the commonly employed continuous stiffness measurement technique (CSM) because of the “plasticity error” recently reported by Merle et al. [Acta Mater.134, 167 (2017)]. To circumvent this problem, here we explore an alternative testing and analysis procedure based on quasi-static loading and an independent knowledge of the Young's modulus, which is easily obtained by standard nanoindentation testing. In theory, the method applies to any indentation strain rate, but in practice, an upper limit on the rate arises from hardware limitations in the testing system. The new methodology is developed and applied to measurements made with an iMicro nanoindenter (KLA, Inc.), in which strain rates up to 100 s−1 were successfully achieved. The origins of the hardware limitations are documented and discussed.

Nanoindentation and microcrystal deformation are two methods that allow probing size effects in crystal plasticity. In many cases of microcrystal deformation, scale-free and potentially universal intermittency of event sizes during plastic flow has been revealed, whereas nanoindentation has been mainly used to assess the stress statistics of the first pop-in. Here, we show that both methods of deformation exhibit fundamentally different event-size statistics obtained from plastic instabilities. Nanoindentation results in scale-dependent intermittent microplasticity best described by Weibull statistics (stress and magnitude of the first pop-in) and lognormal statistics (magnitude of higher-order pop-ins). In contrast, finite-volume microcrystal deformation of the same material exhibits microplastic event-size intermittency of truncated power-law type even when the same plastic volume as in nanoindentation is probed. Furthermore, we successfully test a previously proposed extreme-value statistics model that relates the average first critical stress to the shape and scale parameter of the underlying Weibull distribution.

This study explores magnetization exhibited by nanoscale platinum-based structures embedded in pure silica plates. A superposition of laser pulses in the samples produced periodic linear arrangements of micro-sized structures. The samples were integrated by PtO2 microstructures (PtOΣs) with dispersed Pt oxide nanoparticles in their surroundings. The characterization of the materials was performed by high transmission electron microscopy studies. Furthermore, topographical and magnetic effects on the sample surfaces were analyzed by atomic force microscopy and magnetic force microscopy, respectively. The magnetic measurements indicated an enhancement in the gradient phase shift and in the gradient force related to the magnetic PtOΣs. The possibility of tuning the magnetic characteristics of the samples through contact with a Nd2Fe14B magnet was demonstrated. This process corresponds to an innovative method for obtaining magnetic PtOΣs induced by laser pulses. Moreover, an increase in the compactness of the silica with platinum-based structures was confirmed by an evaluation of the effective elastic modulus with reference to pure silica. The multimodal magnetic structures studied in this work seem to be candidates for developing high-density magnetic storage media.

Measuring the elastic and plastic properties with nanoindentation is predicated on the indentation not fracturing the material. In this study, an unloading curve analysis is used to identify indentation-induced fracture in brittle molecular organic crystals to define conditions, where properties measurements are accurate, and for calculating the toughness. Single crystals of cyclotetramethylene tetranitramine (HMX) and idoxuridine were indented from 1 to 300 mN with indenter probes of varying acuity to identify fracture initiation loads. Idoxuridine displayed no fracture up to and at 100 mN, with fracture occurrence then seen at an increasing rate until every indentation made induced fracture at 300 mN. HMX displayed no fracture up to and at 4 mN, with fracture then occurring at an increasing rate until every sample fractured at 8 mN. The toughness of HMX and idoxuridine is ≈0.28 ≈ 0.4–0.5 MPa/m1/2, respectively.

Under electrochemical cycling, stress intensification and relaxation within small volumes at the lithium/solid-state electrolyte (SSE) interface are thought to be critical factors contributing to mechanical failure of the SSE and subsequent short-circuiting of the device. Nanoindentation has been used to examine the diffusion-limited pressure lithium can support in the absence of active dislocation sources at high homologous temperatures. Based on the underlying physics of this deformation mechanism, a simple perturbation model coupling local current density, elastic stress, and diffusional creep relaxation is introduced. Combining this analysis with the indentation results, it is possible to describe a defect length scale which is too large for effective diffusional creep relaxation, but too small for efficient dislocation multiplication. In this instance, the properties of the SSE may become critical, and relevant indentation results of the SSE are described. The final outcome of the proposed analysis is a newly developed deformation mechanism map.

Constant strain rate nanoindentation is a popular technique for probing the local mechanical properties of materials but is usually restricted to strain rates ≤0.1 s−1. Faster indentation potentially results in an overestimation of the hardness because of the plasticity error associated with the continuous stiffness measurement (CSM) method. This can have significant consequences in some applications, such as the measurement of strain rate sensitivity. The experimental strain rate range can be extended by increasing the harmonic frequency of the CSM oscillation. However, with commercial instruments, this is achievable only by identifying higher CSM frequencies at which the testing system is dynamically well behaved. Using these principles, a commercial system operated at the unusually high harmonic frequency of 1570 Hz was successfully used to characterize of the strain rate sensitivity of a Zn22Al superplastic alloy at strain rates up to 1 s−1, i.e., an order of magnitude higher than with standard methods.

An analysis of indentation cyclic behavior of polymers is carried out with the aim to tackle time-dependent behavior of polymer at several time scales by one test. The method consists in cycling the load between a positive close-to-zero value and a maximum peak value (10 mN in this study) for long time with constant loading rate. The short time scale is characterized through the instantaneous elastic modulus determined from reloading curves at each cycle. The advantages of determination of instantaneous elastic modulus from reloading instead of commonly used unloading curves are discussed. The energy dissipation describes viscoelasticity and plasticity at the time scale of one cycle. The evolution of both parameters with cycles along with the cyclic creep describes the long-time viscoelasticity. The cyclic indentation behavior of poly(methyl methacrylate), PR520 epoxy, and high-density polyethylene (HDPE) polymers is analyzed, and a comparison with the macroscopic cyclic behavior of HDPE is presented.

A major limitation in nanoindentation analysis techniques is the inability to accurately quantify pile-up/sink-in around indentations. In this work, the contact area during indentation is determined simultaneously using both contact mechanical models and direct in situ observation in the scanning electron microscope. The pile-up around indentations in materials with low H/E ratios (nanocrystalline nickel and ultrafine-grained aluminum) and the sink-in around a material with a high H/E ratio (fused silica) were quantified and compared to existing indentation analyses. The in situ projected contact area measured by Scanning Electron Microscopy using a cube-corner tip differs significantly from the classical models for materials with low H/E modulus ratio. Using a Berkovich tip, the in situ contact area is in good agreement with the contact model suggested by Loubet et al. for materials with low H/E ratio and in good agreement with the Oliver and Pharr model for materials with high H/E ratio.

The basis of the virtual machine concept, which is commonly used in coordinate measuring machines, was implemented to determine more realistic uncertainties on the estimation of the elastic modulus obtained from nanoindentation tests. The methodology is based on a mathematical model applied to simulate the testing process and to evaluate the uncertainties through Monte Carlo simulations whose application depends on the studied system (instrument, material, scale, etc.). The methodology was applied to the study of fused silica (FQ) and steel samples tested in a nanoindentation system. The results revealed that the most relevant sources of uncertainty are related to the calibration procedure, particularly to the elastic modulus of the calibration material, and to the contact depth estimation; however, the relevance of the uncertainties is system dependent. This work represents a first insight for a deeper consideration of the uncertainties in instrumented indentation testing.