Search

The combination of conventional physical vapor deposition and a gas aggregation nanoparticle source enabled the study of model systems of unique material combinations and dimensions. Zr50Cu45Ag5 thin film metallic glasses with varying contents of single-crystalline 5 nm tungsten nanoparticles were synthesized using this technique. This approach provides precise control over nanoparticle shape, size, distribution, and concentration. The films were later annealed at 150 °C, 250 °C, 350 °C, and 450 °C. At room temperature inclusion of 0.01 vol% tungsten nanoparticles caused a 15% increase in the nanoindentation hardness of a thin film metallic glass, while having no significant effect on pop-in length or frequency, as seen in the loading curves. Even more remarkably, at 450 °C a control film containing no nanoparticles experienced significant segregation and subsequent crystallization, whereas this effect was repressed in the tungsten nanoparticle composite thin film metallic glass. Unobstructed by nanoparticles, at high temperatures zirconium diffused to the surface of the film, forming a crystalline layer of up to 80 nm. In contrast, this layer is kept to below 30 nm when the nanoparticles are present. The stabilization of the microstructure is also clear from indentation results, while the hardness of the reference sample changes significantly due to the undesired crystallization, the hardness of the composite remains constant., Thin Solid Films, 773, ISSN:0040-6090, ISSN:1879-2731

The effect of length scale on mechanical strength is a significant consideration for semiconductor materials. In III-V semiconductors, such as InSb, a transition from partial to perfect dislocations occurs at the brittle-to-ductile transition temperature (~150 °C for InSb). High temperature micro-compression reveals InSb to show a small size effect below the transition, similar to ceramics, while in the ductile regime it shows a size effect consistent with fcc metals. The source truncation model is found to agree with the observed trends in strength with size once the change in Burgers vector and bulk strength are taken into account.

A composition-spread Cu-Zr thin film library with Zr contents from 2.5 up to 6.5 at.% was synthesized by magnetron sputtering on a thermally oxidized Si wafer. The compositional and microstructural variations of the Cu-Zr thin film across the composition gradient were examined using energy dispersive X-ray spectroscopy, X-ray diffraction, and high-resolution scanning and transmission electron microscopy of cross-sections fabricated by focused ion beam milling. Composition-dependent hardness and elastic modulus values were obtained by nanoindentation for measurement areas with discrete Zr contents along the composition gradient. Similarly, the electrical resistivity was investigated by 4-point resistivity measurements to study the influence of Zr composition and microstructural changes in the thin film. Both, the mechanical and electrical properties reveal a significant increase in hardness and resistivity with increasing Zr content. The trends of the mechanical and functional properties are discussed with respect to the local microstructure and composition of the thin film library.

Micro- and nanomechanical testing has seen a rapid development over the last decade with miniaturized test rigs and MEMS-based devices providing access to the mechanical properties and performance of materials from the micrometer down to the tenths of nanometer length scale. In this overview, we summarize firstly the different testing concepts with excursions into recent imaging and diffraction developments, which turn micro- and nanomechanical testing into “quantitative mechanical microscopy” by resolving the underlying material physics and simultaneously providing mechanical properties. A special focus is laid on the pitfalls of micro-compression testing with its stringent boundary conditions often hampering reliable experiments. Additionally, the challenges of instrumented micro- and nanomechanical testing at elevated temperature are summarized. From the wide variety of research topics employing micro- and nanomechanical testing of materials we focus here on miniaturized samples and test rigs and provide three examples to elucidate the state-of-the-art of the field: (i) probing the “strength” of individual grain boundaries in metals, (ii) temperature dependent deformation mechanisms in metallic nanolayered and -alloyed structures, and (iii) the prospects and challenges of fracture studies employing micro- and nanomechanical testing of brittle and ductile monolithic materials, and materials containing interfaces. Proven concepts and new endeavors are reported for the topics discussed in this overview.

A combinatorial science approach is utilized to study the microstructural and mechanical properties of metastable copper‑tungsten solid solutions. Lateral compositional gradient (also called composition-spread) samples were deposited by simultaneously sputtering copper and tungsten targets positioned obliquely at opposite ends of a silicon substrate. The chemical composition of the film varies continuously along its length from 12 to 45 atomic % copper and has a nominal thickness of 1 μm. Nanoindentation was performed to measure the hardness and elastic modulus of the film. Grain size and solid solution strengthening models are applied to interpret the hardness of the film, though a simple rule of mixtures is found to give a more satisfactory fit to the data. The elastic modulus of the film is consistently below that predicted by the rule of mixtures. X-ray diffraction revealed plane spacing less than that predicted by Vegard's law as well as three chemical compositions exhibiting enhanced long-range order. Transmission electron microscopy analysis confirms that the film consists of a single metastable body centred cubic solid solution where the lattice spacing and grain size depend on chemical composition.

The size dependence of the mechanical behavior of a single crystalline equiatomic FeCrCoMnNi single phase high entropy alloy was studied using in situ SEM microcompression. Electron back-scattered diffraction was used in conjunction with high-resolution scanning electron microscopy to identify the dominant slip system activated for accommodating plastic flow. The scaling of the yield strength with the size of the micropillar is discussed in comparison with the size dependence observed in face-centered and body-centered cubic single crystalline metals.

Based on a combination of micropillar compression experiments and modelling of the secondary cell wall (cw) using continuum micromechanics, the shear yield stress of the polymer matrix is identified for both normal and compression wood of Norway spruce. It is shown that the model is able to capture the differences in mechanical properties between the two tissues based on the knowledge of composition of the samples, microfibril angle, as well as phase properties on the nanometer scale. By testing an isolated piece of the cell wall with a homogeneous and uniaxial stress field on the micrometer scale and using the micromechanical model to determine average stress fields on the nanometer scale, it is possible to identify the shear yield stress of the polymer matrix in wood, which was found to be in the range of 14.9–17.5 MPa for normal and compression wood. It was shown that this corresponds to a stress in the lignin phase of approx. 17 MPa. This combined study thus demonstrates a new approach for validating ...

The thermal stability of evaporated copper–chromium alloy films was studied by correlating hardness trends from nanoindentation to nanostructural–compositional changes from transmission electron microscopy. In particular, the hardness evolution with ageing time at ambient and elevated temperatures of two compositions, dilute (Cu96Cr4) and chromium-rich (Cu67Cr33) solutions, was studied. Due to the negligible mutual miscibility of copper and chromium, the chosen solid solutions are trapped in metastable states as supersaturated solid solutions with face-centred cubic and body-centred cubic phases. Nano-mechanical probing of the nanostructural evolution as a function of temperature provided interesting insights into the phase separation of these systems.

The mechanical behavior of Cu–Cr nanolayered films and an alloy film of nominal composition Cu 20 Cr 80 at.% was studied by microcompression testing at temperatures from 25 °C to 300 °C. Comparing nanolayered films, plastic deformation and failure occurred at consistently higher stress levels in the film with the smaller layer thicknesses. Plasticity in the nanolayered films always initiated in the softer Cu layers followed by a finite strain-hardening response in the stress–strain curves. Failure indicated by a strain-softening response following the higher peak strength due to shearing and tearing at columnar boundaries of Cr was observed in the nanolayered films at 25 °C and 100 °C. A transition from shearing and crack formation across the Cu–Cr interfaces leading to anomalous grain growth or beading of the nanocrystalline Cu layers was observed at elevated temperatures of 200 °C and 300 °C. On the other hand, the Cu 20 Cr 80 at.% alloy film exhibited failure by columnar buckling consistently at elevated temperatures, but shearing promoted by buckling at the highest strengths among the films at ambient temperature.

The microthermomechanical behavior of a precipitation-hardenable Ni-48Ti-25Pd (at.%) shape memory alloy has been investigated as a function of temperature. Micropillars were fabricated within a large 〈145〉-oriented grain and compressed in situ in the SEM at elevated temperatures corresponding to the martensite and austenite phase transformation temperatures. The precipitation-strengthened alloys exhibited stable pseudoelastic behavior with little or no residual strains when near the transformation temperatures. In the plastic regime, slip was observed to occur via pencil glide, circumventing the fine scale precipitates along multiple slip planes.

The yield strengths and deformation mechanisms of Cu–Cr nanolayered and alloyed thin films were studied by microcompression testing at elevated temperatures. The mechanical response of the films with alternating layers of Cu and Cr with sub-100 nm interlayer thicknesses and alloyed films of the same average composition was compared to determine the role of the interfaces on deformation. Higher resistance to plastic flow at elevated temperatures was exhibited by the nanolayered films with smaller interlayer thickness among the layered films, while the alloyed film revealed an anomalous increase in strength with temperature exhibiting a deformation mechanism similar to the pure Cr film.

Nanolaminates of Cu and W with a bilayer thickness ratio of 1:1 and individual layer thicknesses of 5, 20 and 100 nm were studied by using elevated temperature microcompression. Failure in all the multilayers with different interlayer thicknesses occurs by rupture of the W interlayers, resulting in local strain softening and shearing at ambient temperature and lateral plastic flow of the Cu layers confined between the harder W layers at lower stresses with increasing testing temperatures.

The mechanical properties and deformation mechanisms of nano-porous ZnO thin films electrodeposited on glass substrates were determined by nanoindentation and in situ scanning electron microscope (SEM) micropillar compression. The intragranular nature of the nanoscale porosity within the individual mono-crystals of the films was probed at nano- and micro-scales for determining their mechanical response. The hardness (3.5 GPa) and reduced elastic modulus (65 GPa) of the compact thin film were found to decrease by increasing the intragranular porosity controlled by the electrochemical deposition potential of ZnO. Focused ion beam (FIB) cross-sections of residual imprints reveal that the decrease in hardness and elastic modulus observed is primarily due to compaction of the nano-porous structure. In situ SEM compression of FIB machined micropillars reveals brittle fracture and near theoretical strengths in the compact film (~ 2 GPa), and a higher flaw tolerant response despite lower failure stress in the most porous film.

Friction and wear minimizing coatings are crucial for applications in combustion engines and medical implants. Their performance is typically limited by mechanical failure especially due to local overload. In this work, the contact damage creation, evolution, and final morphology of hydrogenated diamond-like carbon (DLC)-coated titanium (Ti) substrates are investigated. The influence of the DLC film thickness and the elastic–plastic deformation of the Ti on the contact damage are studied by microindentation and static finite-element analysis. Film thickness, indenter radius, and applied load as well as the elastic–plastic deformation of the Ti are shown to significantly affect contact damage. A failure plot is presented with the location of first failure in the DLC and compared to the experimental observation. In addition, a case study with variable fracture toughness of the DLC and its influence on the failure plot is shown. The stress distribution in the DLC follows a transition from a membrane-like to a plate-like deformation behavior upon increasing the DLC film thickness. Thin DLC films reveal increased cracking in the inner zone of the indent, while thicker DLC films reveal pronounced edge cracking. These edge cracks were correlated to pop-ins in force–displacement curves upon microindentation. Finally, a film thickness optimization process is presented for hard and brittle films on soft and ductile metallic substrates.

The deformation and failure mechanism of a multilayered thin film consisting of alternating soft Cu and hard TiN interlayers has been studied by in situ SEM compression of micro-pillars and finite element simulations. While the yielding of the multilayer is governed by the 'size-dependent' strength of Cu, the failure was found to occur by shearing of the columnar grains of TiN. At elevated temperatures of 200 and 400 °C, the yielding of the multilayers is governed by the stress-assisted diffusion of the Cu interlayers, which coalesce into microcrystals and grow into larger faceted crystals.

Metastable binary Cu–Cr alloys with nominal film thicknesses of 300 nm and chemical compositions in the range of 4–93 at.% Cr were synthesized via co-evaporation using molecular beam epitaxy. All films were grown onto Si (1 0 0) substrates at deposition rates of ∼0.05 nm s−1. The film microstructures were studied by using transmission electron microscopy and X-ray diffraction. The mechanical properties were investigated by the nanoindentation technique. Depending on the chemical composition, three types of thin film microstructures are observed, which all exhibit tensile residual stresses. For a Cr concentration of 4 at.% a single-phase face-centered cubic (fcc) film was formed, whereas single-phase body-centered cubic (bcc) films were observed for Cr concentrations ⩾ 33 at.%. In the case of a Cu85Cr15 film, a two-phase fcc and bcc structure is formed. An increase of the atomic fraction of Cr induces a significant refinement of grain sizes, from ∼100 nm for a Cu96Cr4 alloy to ∼30 nm in the case of a Cu20Cr80 alloy. Consequently, the hardness of the alloy films increased from 5.5 to 11.8 GPa. In addition, the formation of supersaturated solid solutions of Cr in single-phase fcc Cu films and Cu in single-phase bcc films was observed. Predictions of existing models of solid solution and grain boundary strengthening were evaluated and correlated with the mechanical properties of the films with respect to film compositions and grain sizes.

Diamond ⟨100⟩- and ⟨111⟩-oriented nanopillars were fabricated by focused ion beam (FIB) milling from synthetic single crystals and compressed using a larger diameter diamond punch. Uniaxial compressive failure was observed via fracture with a plateau in maximum stress of ∼0.25 TPa, the highest uniaxial strength yet measured. This corresponded to maximum shear stresses that converged toward 75 GPa or ∼ G/7 at small sizes, which are very close to the ultimate theoretical yield stress estimate of G/2π.

Nanocrystalline and ultrafine-grained materials show enhanced strain rate sensitivity (SRS) in comparison to their coarse grained counterparts. Majority of SRS measurements on nanocrystalline thin films reported in literature have focused on nanoindentation-based approaches. In this paper, micropillar strain rate jump tests were demonstrated on an electrodeposited nanocrystalline nickel film from 25 to 100 °C. SRS exponent, m, and activation volume, V, values were determined as a function of temperature. The measured values were found to be in good agreement with previously reported literature on bulk and nanoindentation measurements. Apparent activation energy for deformation was found to be about 100 kJ/mol, which is close to that for grain boundary diffusion in nickel. Grain boundary sliding was observed in the deformed pillars from scanning electron microscopy images.

By designing advantageous cellular geometries and combining the material size effects at the nanometer scale, lightweight hybrid microarchitectured materials with tailored structural properties are achieved. Prior studies reported the mechanical properties of high strength cellular ceramic composites, obtained by atomic layer deposition. However, few studies have examined the properties of similar structures with metal coatings. To determine the mechanical performance of polymer cellular structures reinforced with a metal coating, 3D laser lithography and electroless deposition of an amorphous layer of nickel-boron (NiB) is used for the first time to produce metal/polymer hybrid structures. In this work, the mechanical response of microarchitectured structures is investigated with an emphasis on the effects of the architecture and the amorphous NiB thickness on their deformation mechanisms and energy absorption capability. Microcompression experiments show an enhancement of the mechanical properties with the NiB thickness, suggesting that the deformation mechanism and the buckling behavior are controlled by the brittle-to-ductile transition in the NiB layer. In addition, the energy absorption properties demonstrate the possibility of tuning the energy absorption efficiency with adequate designs. These findings suggest that microarchitectured metal/polymer hybrid structures are effective in producing materials with unique property combinations.