Studies on the mechanics of plant cells usually focus on understanding the effects of turgor pressure and properties of the cell wall (CW). While the functional roles of the underlying cytoskeleton have been studied, the extent to which it contributes to the mechanical properties of cells is not elucidated. Here, we study the contributions of the CW, microtubules (MTs) and actin filaments (AFs), in the mechanical properties of Nicotiana tabacum cells. We use a multiscale biomechanical assay comprised of atomic force microscopy and micro-indentation in solutions that (i) remove MTs and AFs and (ii) alter osmotic pressures in the cells. To compare measurements obtained by the two mechanical tests, we develop two generative statistical models to describe the cell’s behaviour using one or both datasets. Our results illustrate that MTs and AFs contribute significantly to cell stiffness and dissipated energy, while confirming the dominant role of turgor pressure.

A new constant contact pressure (CCP) indentation creep method is presented, which is based on keeping the mean contact pressure as defined through Sneddon’s hardness constant, until a steady-state strain rate is achieved. This is in contrast to the conventional constant load–hold (CLH) creep experiments, where the load is held constant and relaxation in both hardness and strain rate occurs at the same time. Besides controlling the mean contact pressure, the dynamic stiffness is furthermore used to assess the indentation depth, thereby minimizing thermal drift influence and pile-up or sink-in effects during long-term experiments. The CCP method has been tested on strain rate sensitive ultrafine-grained (UFG) CuZn30 and UFG CuZn5 as well as on fused silica, comparing the results with those of strain rate jump tests as well as the CLH nanoindentation creep tests. With the CCP method, strain rates from 5 × 10−4 s−1 down to 5 × 10−6 s−1 can be achieved, keeping the mean contact pressure constant over a long period of time, in contrast to the CLH method. The CCP technique thus offers the possibility of performing long-term creep experiments while retaining the contact stress underneath the tip constant.

The high precision offered by small-scale mechanical testing has allowed the relationships between mechanical behavior and specific microstructural features to be determined to an unprecedented degree. However, of most interest to scientists and engineers is often the behavior of materials under service conditions in an extreme environment, such as high/low temperatures, high strain rates, hydrogen atmosphere, or radiation. In this article, we detail progress made to adapt nanomechanical testing systems and techniques to observe materials behavior in situ in extreme environments.

The extrinsic indentation size effect (ISE) is utilized to analyze the depth-dependent hardness for Berkovich indentation of non-uniform dislocation distributions with one and two dimensional deformation gradients and is then extended to indentation results at grain boundaries. The role of the Berkovich pyramid orientation and placement relative to the grain boundary on extrinsic ISE is considered in terms of slip transmission at yield and plastic incompatibility during post-yield deformation. The results are interpreted using a local dislocation hardening mechanism originally proposed by Ashby, combined with the Hall–Petch equation. The Hall–Petch coefficient determined from the extrinsic ISE of the grain boundary is found to be consistent with the published values for pure Fe and mild steel. A simple, linear continuum strain gradient plasticity model is used to further analyze the results to include contributions from a non-uniform distribution in plastic strain and dislocation density.

In our previous study, we observed a lack of $\left\{ {10\bar{1}2} \right\}$ twinning in a deformed Mg–Y alloy, which contributed to the observed yield “symmetry.” However, the effects of texture and grain size on polycrystalline deformation made it difficult to fully understand why twinning was not active. Therefore, we report herein in-depth study by in situ transmission electron microscopy, i.e., in situ TEM. The in situ deformation of nano-sized Mg–Y pillars revealed that prismatic slip was favored over twinning, namely, the critical stress required to activate prismatic slip was lower than that for twinning. This finding diametrically differs from that reported in other nano/micro-pillar deformation studies, where twinning is always the dominant deformation mechanism. By measuring the critical stresses for basal, prismatic, and pyramidal slip systems, this in situ TEM study also sheds light on the effects of the alloying element Y on reducing the intrinsic plastic anisotropy in the Mg matrix.

A fracture analysis is developed for crack initiation sequences occurring during sharp indentation of brittle materials. Such indentations, generated by pyramidal or conical loading, generate elastic and plastic deformation. The analysis uses a nonlinear elements-in-series model to describe indentation load–displacement responses, onto which lateral, radial, cone, and median crack initiation points are located. The crack initiation points are determined by extension and application of a contact stress-field model coupled to the indentation load, originally developed by Yoffe, in combination with crack nuclei coupled to the indentation displacement to arrive at an explicit fracture model. Parameters in the analysis are adapted directly from experimental fracture and deformation measurements, and the analysis outputs are directly comparable to experimental observations. After adaptation, crack initiation loads and sequences during indentation loading and unloading of glasses and crystals are predicted by the model from material modulus, hardness, and toughness values to within about 25% of peak contact load. This work is dedicated to George M. Pharr IV on the occasion of his 65th birthday in recognition of his contributions to indentation mechanics.

Concurrently assessing localized residual stresses and mechanical properties in cases where there are gradients in stresses and properties (such as those resulting in metallic alloys from shot peening processes) is challenging. Most indentation-based stress measurements assume uniform properties, which is not necessarily the case in this common industrial process. By using the energy envelope describing the total work of indentation by a load–displacement curve from instrumented indentation, localized residual stresses after shot peening were evaluated experimentally. A framework is developed to describe the appropriate indentation depth at which to assess properties that effectively define the volumetric resolution of the method. The residual stresses predicted via the nanoindentation experiment and energy analysis were validated with X-ray measurement of residual stresses on a shot-peened 52100 steel. The energy method can be applied directly from the indentation load–displacement curve without considering the contact area.

A high-temperature nanoindentation system was used to examine the steady state indentation creep behavior of CsHSO4. This high proton conductivity solid-acid material is a candidate for use as a solid-state electrolyte in intermediate temperature fuel cells. Constant strain rate indentation creep tests yielded a stress exponent and a creep activation energy in close agreement with results obtained from previous uniaxial compression testing. The large penetration depths reached during creep testing necessitated validating an indenter area function well beyond depths measurable in fused silica. The developed methodology is material agnostic meaning it can be used for indentation creep measurements in other high creep rate materials. In addition, it is shown how an analysis developed by Bower et al. (Proc. Royal Soc. 441, 97–124, 1993) can be successfully used to convert the indentation creep parameters into the more common material parameters measured in uniaxial creep tests.

Residual stress is generally evaluated using indentation by comparing the indentation curves of stressed and stress-free states. Here, we suggest a new method that can evaluate surface residual stress without indentation testing on stress-free specimen using stress-independent indentation parameters and an analysis of indentation contact morphology for the stress-free state. We found that several indentation parameters are independent of the stress by Vickers indentation testing on various stress states. The indentation contact morphology can be represented by indentation parameters including stress-independent ones, and by applying the stress-independent parameters obtained from the stressed state to the indentation contact depth function, we can estimate an indentation curve for stress-free state. The estimated curve matches well with the experimental stress-free indentation curve, and it was also confirmed that the applied stress values evaluated by comparing the estimated curve with the stressed indentation curve agree well with the reference values obtained from strain gauge.

The mechanical properties of metallic glasses are often tuned by annealing, which influences these properties by adjusting the relaxation and/or crystallization status of the glasses. Here, we studied the hardness and modulus of Pt57.5Cu14.7Ni5.3P22.5 bulk metallic glass annealed at different temperatures by nanoindentation, where the annealing gives the material different fictive temperatures and fractions of crystallization. It is found that both reducing the fictive temperature of a fully amorphous sample and increasing the degree of crystallization in a partially crystallized sample increase hardness and modulus. Combining the two approaches, elevated hardness and modulus values are found for composite materials containing both crystalline and amorphous phases when they are compared to chemically identical alloys featuring similar percentages of crystalline and amorphous phases that have been prepared by annealing at higher temperatures. Our findings indicate that the mechanical properties of the platinum-based alloys can be customized by processing them with targeted heat treatments.

Polyurea resins derived from tolyldiisocyante (TDI) and a reactive solvent-free nanofluid (NF-NH2) surface-decorated with propylamines can be tuned over three to five orders of magnitude in storage modulus (10 MPa to 10 GPa) and hardness modulus (6 kPa to 4 GPa) by varying weight fractions of components. The thermal properties of this NF-NH2 are similar to several other nanofluids reported using the same bulky anionic counterion that also imparts liquidity in the absence of any solvent. This tuning suggests applications ranging from opaque protective coatings to clearcoats to sealants to adhesives.

Polydopamine (PDA) is a biopolymer, which can form uniform thin films on almost all solid substrates as well as at the liquid/air interface. Carbonized polydopamine possesses graphite-like structure and exhibits high electrical conductivity, which makes it a potential carbon-based thin film conductor. However, studies on mechanical behavior of PDA and its derived materials are very limited. In this study, PDA samples were synthesized through self-assembly of dopamine in aqueous solution. Elastic modulus of thin films was measured using the nanoindentation technique. It is shown that the Young’s modulus of PDA thin film increased with increasing heat treatment temperature (up to 600°C). Doping with Cu ions also increased the Young’s modulus of PDA. Furthermore, all PDA thin films, with and without Cu, exhibited creep behavior.

Sintered tape-cast yttria-stabilized zirconia (YSZ) was evaluated for its elemental composition, crystal structure, and imaged with atomic force microscopy (AFM) and scanning electron microscopy (SEM). Human bone marrow stem cells (hBMSC) were cultured on the ceramic and differentiated into the osteoblast lineage; alkaline phosphatase (ALP) activity was tracked as a differentiation marker. The YSZ was composed of purely tetragonal grains with a median equivalent circular diameter of 283 nm. Zirconium, yttrium, oxygen, and adventitious carbon was detected on the substrate with no other elements in significant quantities detected. YSZ samples had an RMS roughness value of 27 nm, elastic modulus of 206 ± 14 GPa, and hardness of 14 ± 2 GPa. hBMSC were observed to attach and proliferate on the YSZ surfaces and had significantly increased ALP versus the undifferentiated control cultured on glass. This method for producing a YSZ ceramic yields a typical material of this type and supports attachment and differentiation of hBMSC; thus, making it useful as a bone implant material.

It is well known that various elements substitute for a certain sub-lattice of intermetallic compounds. There have been various experimental investigations of the effects of substituted elements on mechanical properties, however, there are few reports describing the effects of multi-element substitution. In the present study, L12-type compounds A3B (Ni3Al and Co3(Al,W)) were selected as model compounds because their substitution behavior is well known. It was reported that various elements such as Ni, Co, Cu, Pd and Pt occupy the A-site, whereas Al, Si, Ga, Ge, Ti, V, Nb, Ta, Mo, and W occupy the B-site. These elements are expected to introduce local lattice distortion, which may affect the motion of dislocations over a wide range of temperatures. Several alloys composed of five or more elements including Ni, Co, Al, Mo, and W, were prepared using an Ar-arc melting machine and heat-treated. Several alloys were found to include an (Ni, Co)3(Al, Mo, W, …)-L12 compound as a constituent phase. The nano-hardness of these L12 phases was higher than that of the high-strength Co3(Al,W)-L12 compound, confirming that multi-element substitution is an effective way to improve the mechanical properties of an intermetallic compound without decreasing the phase stability.

Brachiopods are a phylum of shell-forming sessile marine invertebrates which have existed since the early Cambrian. Two very different biomaterial design strategies for their shells evolved early in their history. Both strategies use hybrid fibre composites, however, one is based on mineral fibres embedded in ~2 wt.% of organic biopolymer sheaths and the inorganic fibres are calcite single crystals. In the second strategy the fibres are biopolymers and are reinforced with Ca-phosphate nanoparticles to form a fibrous nanocomposite. Here the organic component (chitin) dominates. The Ca-phosphate nanoparticle-reinforcement strategy is not unlike that in vertebrate bone, however, the microscale structure is laminated with alternating laminae which have a different degree of mineralization.

The calcitic shells feature an outer compact layer of calcite micro- and nanoparticles protecting the inner fibrous layer from the outside. Transmission electron microscopy of the fibrous layer reveals intercrystalline and intracrystalline biopolymers. The calcitic shell material is stiff with nano-indentation E-moduli of 63±8 GPa and relatively hard (Vickers microhardness up to 400 HV 0.0005/10 and nanohardness 4±0.5 GPa). Compared to inorganic calcite the microhardness is doubled and the nanohardness increases by 60%. We attribute this increased hardness to intracrystalline biopolymers. The nano-indentation E-moduli of the chitinophosphatic shells range from 3 to 55 GPa as a result of the varying degree of mineralization between their laminae, and similarly their nanohardness varies between 0.1 and 3 GPa. For brachiopods burrowing inside the sediment, the alternation of non-mineralized laminae with thin, more strongly mineralized laminae provides abrasion-resistance, hardness and longitudinal stiffness while it preserves the flexibility provided by the organic component for bending movements.

Calcium carbonate biominerals are frequently analysed in materials science due to their abundance, diversity and unique material properties. Aragonite nacre is intensively studied, but less information is available about the material properties of biogenic calcite, despite its occurrence in a wide range of structures in different organisms. In particular, there is insufficient knowledge about how preferential crystallographic orientations influence these material properties. Here, we study the influence of crystallography on material properties in calcite semi-nacre and fibres of brachiopod shells using nanoindentation and electron backscatter diffraction (EBSD). The nano-indentation results show that calcite semi-nacre is a harder and stiffer (H ≈ 3—5 GPa; E = 50–85 GPa) biomineral structure than calcite fibres (H = 0.4—3 GPa; E = 30—60 GPa). The integration of EBSD to these studies has revealed a relationship between the crystallography and material properties at high spatial resolution for calcite semi-nacre. The presence of crystals with the c-axis perpendicular to the plane-of-view in longitudinal section increases hardness and stiffness. The present study determines how nano-indentation and EBSD can be combined to provide a detailed understanding of biomineral structures and their analysis for application in materials science.

Nanoindentation has been used to measure the elastic modulus of 5 and 18 μm thick high-purity vapor deposited polycrystalline lithium films at 31 °C. Over indentation depths ranging from 150 to 1100 nm, the modulus is found to vary with film thickness from 9.8 GPa ± 11.9% to 8.2 GPa ± 14.5%. These results are well within the range of lithium's orientation dependent elastic modulus, which spans approximately 3.1 to 21.4 GPa. The measured values may also indicate (111) and (100) texture for the 5 and 18 μm thick films, respectively. The potential effects of pileup and surface contamination are found to be negligible if any at all. Small but discernible changes in damping capability near the free surface may provide insight into the subsurface defect structure and the potential for localized heating. Numerous experimental challenges are addressed and key metrics are used to validate the measured elastic modulus.

We present a method for measuring the shear complex modulus of hydrogels by oscillatory nanoindentation, with unprecedented attention to procedure and uncertainty analysis. The method is verified by testing a typical low-molecular-weight gelator formed from the controlled hydrolysis of glucono-δ-lactone. Nanoindentation results are compared with those obtained by rheometry using both vane-in-cup and parallel-plate fixtures. At 10 Hz, the properties measured by oscillatory nanoindentation were G′ = 38.1 ± 2.8 kPa, tan δ = 0.22 ± 0.02. At the same frequency, the properties measured by rheometry were G′ = 15.3 ± 2.9 kPa, tan δ = 0.11 ± 0.016 (vane-in-cup) and G′ = 7.9 ± 1.1 kPa, tan δ = 0.05 ± 0.004 (parallel-plate). The larger shear modulus measured by nanoindentation is due to the scale of testing. Whereas rheometry characterizes the bulk material response, nanoindentation probes the fibrous network of the gel. The procedure and analysis presented here are valuable for nanoindentation testing of other compliant materials such as hydrogels, soft biological tissue, and food products.

Ceramic fiber–matrix composites (CFMCs) are exciting materials for engineering applications in extreme environments. By integrating ceramic fibers within a ceramic matrix, CFMCs allow an intrinsically brittle material to exhibit sufficient structural toughness for use in gas turbines and nuclear reactors. Chemical stability under high temperature and irradiation coupled with high specific strength make these materials unique and increasingly popular in extreme settings. This paper first offers a review of the importance and growing body of research on fiber–matrix interfaces as they relate to composite toughening mechanisms. Second, micropillar compression is explored experimentally as a high-fidelity method for extracting interface properties compared with traditional fiber push-out testing. Three significant interface properties that govern composite toughening were extracted. For a 50-nm-pyrolytic carbon interface, the following were observed: a fracture energy release rate of ∼2.5 J/m2, an internal friction coefficient of 0.25 ± 0.04, and a debond shear strength of 266 ± 24 MPa. This research supports micromechanical evaluations as a unique bridge between theoretical physics models for microcrack propagation and empirically driven finite element models for bulk CFMCs.

Characterizing individual ligaments’ behavior during deformation of nanoporous (np) structures remains crucial in further understanding the mechanical response of such materials. In this paper, we report, for the first time, quantifiable results describing the reorientation of ligament structure in np gold (np-Au) subjected to nanoindentation, based on characterization by electron backscatter diffraction (EBSD) orientation mapping. The analysis was performed on a cross-sectioned face at the center of an indent, after specimen preparation utilizing focused ion beam (FIB) techniques. This work provides insights into how the np structure accommodates the material volume displaced during nanoindentation, as well as the strain propagation under the indent. This new knowledge will be fundamental to optimizing utilization of the nanoindentation technique for measurement of np materials and, in particular, np thin films.