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The authors carried out matched experiments and molecular dynamics simulations of the compression of nanopillars prepared from Cu|Au nanolaminates with up to 25 nm layer thickness. The stress–strain behaviors obtained from both techniques are in excellent agreement. Variation in the layer thickness reveals an increase in the strength with a decreasing layer thickness. Pillars fail through the formation of shear bands whose nucleation they trace back to the existence of surface flaws. This combined approach demonstrates the crucial role of contact geometry in controlling the deformation mode and suggests that modulus-matched nanolaminates should be able to suppress strain localization while maintaining controllable strength.
Glassy carbon nanolattices can exhibit very high strength-to-weight ratios as a consequence of their small size and the material properties of the constituent material. Such nanolattices can be fabricated by pyrolysis of polymeric microlattices. To further elucidate the influence of the mechanical size effect of the constituent material, compression tests of glassy carbon nanopillars with varying sizes were performed. Depending on the specific initial polymer material and the nanopillar size, varying mechanical properties were observed. Small nanopillars exhibited elastic-plastic deformation before failure initiation. Moreover, for smaller nanopillars higher strength values were observed than for larger ones, which might be related to smaller defects and a lower defect concentration in the material.
Specifically designed microlattices are able to combine outstanding mechanical and physical properties and, thus, expand the actual limits of the material property space. However, post-yield softening induced by plastic buckling or crushing of individual ligaments limits performance under cyclic loading, which affects their energy absorption capabilities. Understanding deformation under repeated loading is key to further optimizing these high-strength materials. While until now mainly hollow metallic microlattices and multistable or tailored buckling structures have been analyzed, this study investigates deformation and failure of polymer and ceramic-polymer microlattices under cyclic loading to understand the (i) influence of the microarchitecture and (ii) influence of processing conditions on the energy absorption capability. Despite fracture of individual struts, the stretching-dominated microarchitectures possess a superior behavior especially for larger cycle numbers. In combination with a specific annealing treatment of the polymer material, high recoverability and energy dissipation can be achieved.
The effect of Cr fibers on the deformation of directionally solidified NiAl–Cr eutectics, prepared at three different solidification speeds affecting the fiber diameter and fiber spacing, was studied at varying length scales using different micromechanical testing techniques. In situ tensile tests in a scanning electron microscope of individual Cr fibers showed high strength accompanied by ductile behavior. Comparative microcompression tests on single-phase NiAl pillars and NiAl pillars containing a single fiber showed that the pillars with the single fiber were marginally weaker than the single-phase pillars for similar pillar diameters. Composite pillars with multiple fibers exhibited an increase of 0.2% offset strength values with increasing solidification speed. Transmission electron microscopy of the composite pillars containing a single fiber after deformation revealed significant dislocation activity both in the fiber and the matrix. It is argued that the interface between the fiber and matrix acts as dislocation source promoting plastic deformation of the brittle NiAl matrix.
Microcompression test was applied to determine the Young’s modulus for elastically anisotropic materials for two different orientations of single crystalline Si. Although there is a clear difference in the apparent Young’s moduli for the different orientations, a significant underestimation of Young’s modulus was observed resulting from the substrate deformation as observed in both finite element simulation and experiment. This effect decreases with increasing aspect ratio. To correct the deviation of the apparent Young’s modulus from the theoretical values, a systematic framework of microcompression test is suggested. The modified Sneddon correction using the indentation modulus instead of Young’s modulus successfully yields Young’s moduli of single crystalline silicon in the  and  directions to within 5.3% and 2.0% deviation, respectively.
Over the past two decades, nanoindentation has been the most versatile method for mechanical testing at small length scales. Because of large strain gradients, it does not allow for a straightforward identification of material parameters such as yield and tensile strength, though. This represents a major drawback and has led to the development of alternative microscale testing techniques with microcompression as one of the most popular ones today. In this research, the influence of the realistic sample configuration and unavoidable variations in the experimental conditions is studied systematically by combing in-situ microcompression experiments on ultrafine-grained nickel and finite element simulations. It will be demonstrated that neither qualitative let alone quantitative analyses are as straightforward as they may appear, which diminishes the apparent advantages of microcompression testing.
Understanding the finite volume throughout which plastic deformation begins is necessary to understand the mechanics of small-scale deformation. In indentation using spherical indenters, conventional yield criteria predict that yield starts at a point on the axis and at a depth of half the contact radius. However, Jayaweera et al (Proc. Roy. Soc. 2003) concluded that yield occurs over a finite volume at least 100 nm thick. Semiconductor superlattice structures, in which the stress and thickness of individual layers can be varied and in which known internal stresses can be incorporated, open up new possibilities for investigation that cannot be achieved by varying external stresses on a homogenous specimen. We have designed samples with bands of highly strained InGaAs superlattice, which are essentially bands of low yield-stress material devoid of other metallurgical artifacts. These bands are placed at different depths in a series of samples. Spherical indenters with a range of radii were used to determine the elastic-plastic transition. The stress field from different sized indenters interacts with the low yield-stress material at different depths below the surface to map out the size of the initial yield volume.
A new theoretical model is constructed for the viscoelastic response of a clamped circular membrane deformed by a spherical indenter, using the classical Maxwell and Standard Linear Solid (SLS) constitutive equations. Preliminary stress-relaxation experiments are performed for a hydrogel membrane and the corresponding data fitted to the SLS-based viscoelastic model.
It is shown using a method based on the mean field theory of Miklavic Marcelja that it should be possible for osmotic pressure due to the counterions associated with the two polyelectrolyte polymer brush coated surfaces to support a reasonable load (i.e., about 105 Pa) with the brushes held sufficiently far apart to prevent entanglement of polymers belonging to the two brushes, thus avoiding what is likely to be the dominant mechanisms for static and dry friction.
This paper summarises our recent cyclic nanoindentation experiment studies on a range of materials including single crystal and nanocrystalline copper, single crystal aluminium and bulk metallic glasses with different glass transition temperatures. The unloading and reloading processes of the nanoindentation curves have been analysed. The reverse plasticity will be discussed in the context of plastic deformation mechanisms involved. The effect of loading rates on the mechanical properties of materials upon cyclic loading will also be discussed.
The effect of the cobalt content and WC grain size on the deformation behaviour of WC-Co hard metals was investigated by studying materials with a varying WC grain size and cobalt content. The WC grain size ranged from 2.65 to 0.25 µm and the binder content ranged from 6 to 15 wt%. Single and multiple scratch tests were conducted using a Nano indenter with a Berkovich diamond tip and the load ranged from 5 to 500 mN with a tip sliding velocity of 10 µm/s. Several damage mechanisms were observed and these show a combination of ductile and brittle wear. The bulk properties i.e. composite properties of the hard metal determine the wear in the 6 wt% Co samples on the other hand the 15 wt% Co samples exhibited a localised response to the wear i.e. the wear is determined by the individual phases in the hard metal.
There is a technological need for hard thin films with high elastic modulus and fracture toughness. Silicon carbide (SiC) fulfills such requirements for a variety of applications at high temperatures and for high-wear MEMS. A detailed study of the mechanical properties of single crystal and polycrystalline 3C-SiC films grown on Si substrates was performed by means of nanoindentation using a Berkovich diamond tip. The thickness of both the single and polycrystalline SiC films was around 1-2 μm. Under indentation loads below 500 μN both films exhibit Hertzian elastic contact without plastic deformation. The polycrystalline SiC films have an elastic modulus of 457 GPa and hardness of 33.5 GPa, while the single crystalline SiC films elastic modulus and hardness were measured to be 433 GPa and 31.2 GPa, respectively. These results indicate that polycrystalline SiC thin films are more attractive for MEMS applications when compared with the single crystal 3C-SiC, which is promising since growing single crystal 3C-SiC films is more challenging.
In general, the method of obtaining residual stress from indentation test requires calculating the contact area of indenter and indented material, and also needs to know yield stress of indented material in advance. In this work, the dimensional analysis of indentation loading curve was first analyzed, and then a reverse numerical procedure was explored to show a possibility of determining residual stress and yield stress of materials simultaneously from indentation test. Besides, the calculation of contact area can be also avoided.
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 been used to obtain the viscoelastic properties from quasi-static or oscillatory indentations. This paper summarizes our recent findings from modeling indentation in linear viscoelastic solids. These results may help improve methods of measuring viscoelastic properties using instrumented indentation techniques.
Increasingly, indentation creep experiments are being used to characterize rate-sensitive deformation in specimens that, due to small size or high hardness, are difficult to characterize by more conventional methods like uniaxial loading. In the present work we use finite element analysis to simulate indentation creep in a collection of materials whose properties vary across a wide range of hardness, strain rate sensitivities, and work hardening exponents. Our studies reveal that the commonly held assumption that the strain rate sensitivity of the hardness equals that of the flow stress is violated except for materials with low hardness/modulus ratios like soft metals. Another commonly held assumption is that the area of the indent increases with the square of depth during constant load creep. This latter assumption is used in an analysis where the experimenter estimates the increase in indent area (decrease in hardness) during creep based on the change in depth. This assumption is also strongly violated. Fortunately, both violations are easily explained by noting that the “constants” of proportionality relating 1) hardness to flow stress and 2) area to (depth)2 are actually functions of the hardness/modulus ratio. Based upon knowledge of these functions it is possible to accurately calculate 1) the strain rate sensitivity of the flow stress from a measurement of the strain rate sensitivity of the hardness and 2) the power law exponent relating area to depth during constant load creep.
Parallel molecular dynamics simulations were used to study the influence of pre-existing growth twin boundaries on the slip activity of bulk gold under uniaxial compression. The simulations were performed on a 3D, fully periodic simulation box at 300 K with a constant strain rate of 4×107 s−1. Different twin boundary interspacings from 2 nm to 16 nm were investigated. The strength of bulk nano-twinned gold was found to increase as the twin interspacing was decreased. However, strengthening effects related to the twin size were less significant in bulk gold than in gold nanopillars. The atomic analysis of deformation modes at the twin boundary/slip intersection suggested that the mechanisms of interfacial plasticity in nano-twinned gold were different between bulk and nanopillar geometries.
We proposed a method to determine the plastic properties of bulk materials based on data of loading curvature in indentation curve with only one sharp indenter. This method uses the dimensional analysis to solve the representative stress and effective yield stress. Indentation unloading data is only used to select the unique solution from the calculated ones obtained from representative stress and effective yield stress. We applied the proposed method to four engineering metals on an experimental basis, to verify its effectiveness, as well as its superiority to the reported methods.
The thickness and property measurements of thin films on a substrate are crucial for a wide range of applications. Classical techniques have relied on various physical properties to identify film thickness, independent of its mechanical properties. Here, a new experimental technique is devised to evaluate the film thickness, its stiffness and its flow stress. The technique utilizes the variation of the measured apparent modulus of a ductile film on a substrate from a nano-indentation experiment, in conjunction with the measured normal and tangential forces and the scratch depth in a nano-scratch experiment. These combined measurements are calibrated through a simple statically admissible model to yield the unknown quantities. The measurements reasonably agree with the finite element predictions and are ascertained by XPS film thickness measurements. The technique is applied to study the formed oxide nano-layer during copper chemical mechanical planarization process.
In this work we have investigated the strength variability of brittle thin films (thickness ≤ 1 μm) utilising a simple test methodology. Nanoindentation of as-deposited tetrahedral amorphous carbon (ta-C) and Ti-Si-N nanocomposite films on silicon substrates followed by cross-sectional examination of the damage with a Focused Ion Beam (FIB) Miller allows the occurrence of cracking to be assessed in comparison with discontinuities (pop-ins) in the load-displacement curves. Strength is determined from the critical loads at which cracking occurs using the theory of plates on a soft foundation. This is of great relevance, since the fracture strength of thin films ultimately controls their reliable use in a broad range of functional applications.
While elastic and plastic material property extraction from instrumented indentation tests has been well-studied, similarly-based fracture property measurement remains difficult. Furthermore, estimation of the fracture toughness requires measurement of the crack lengths from a micrograph, which makes nano-scale indentation toughness measurement expensive and difficult. Initiation and propagation of cracks on the nano-scale requires a more acute indenter than a Berkovich or sphere, such as the cube-corner pyramid. Experiments described here were performed on a range of elastic, plastic and brittle materials with diamond indenters of acuity varying between the Berkovich and the cube-corner. These experiments reveal some of what is changed and what remains the same, when the acuity of the probe is changed, when fracture is initiated at the contact, or both. A preliminary model for the physical origin of the extra crack-driving power of acute probes is presented in light of these, and complementary macro-scale in-situ indentation experiments. This work provides the basis for development of instrumented indentation-based nano-scale toughness measurement.