Nano Mechanical Testing of Materials and Devices

This study aims to evaluate solder joint reliability under high speed impact tests using nanoindentation properties of intermetallic compounds (IMCs) at the joint interface. Sn–Ag based solder joints with different kinds of interfacial IMCs were obtained through the design of solder alloy/substrate material combinations. Nanoindentation was applied to investigate the mechanical properties of IMCs, including hardness, Young’s modulus, work hardening exponent, yield strength, and plastic ability. Experimental results suggest that nanoindentation responses of IMCs at joint interface definitely dominates joint impact performance. The greater the plastic ability the interfacial IMC exhibits, the superior impact energy the solder joints possess. The concept of mechanical and geometrical discontinuities was also proposed to explain brittle fracture of the solder joints with bi-layer interfacial IMCs subject to impact load. Full article

In this paper, the compressive stress of pristine and coated vertically-aligned (VA) multi-walled (MW) carbon nanotube (CNT) pillars were investigated using flat-punch nano-indentation. VA-MWCNT pillars of various diameters (30–150 µm) grown by low-pressure chemical vapor deposition on silicon wafer. A conformal brittle coating of niobium-titanium-nitride with high superconductivity temperature was deposited on the VA-MWCNT pillars using atomic layer deposition. The coating together with the pillars could form a superconductive vertical interconnect. The indentation tests showed foam-like behavior of pristine CNTs and ceramic-like fracture of conformal coated CNTs. The compressive strength and the elastic modulus for pristine CNTs could be divided into three regimes of linear elastic, oscillatory plateau, and exponential densification. The elastic modulus of pristine CNTs increased for a smaller pillar diameter. The response of the coated VA-MWCNTs depended on the diffusion depth of the coating in the pillar and their elastic modulus increased with pillar diameter due to the higher sidewall area. Tuning the material properties by conformal coating on various diameter pillars enhanced the mechanical performance and the vertical interconnect access (via) reliability. The results could be useful for quantum computing applications that require high-density superconducting vertical interconnects and reliable operation at reduced temperatures. Full article

Size distribution, Young’s moduli and electrical resistivity are investigated for CuO nanowires synthesized by different thermal oxidation methods. Oxidation in dry and wet air were applied for synthesis both with and without an external electrical field. An increased yield of high aspect ratio nanowires with diameters below 100 nm is achieved by combining applied electric field and growth conditions with additional water vapour at the first stage of synthesis. Young’s moduli determined from resonance and bending experiments show similar diameter dependencies and increase above 200 GPa for nanowires with diameters narrower than 50 nm. The nanowires synthesized by simple thermal oxidation possess electrical resistivities about one order of magnitude lower than the nanowires synthesized by electric field assisted approach in wet air. The high aspect ratio, mechanical strength and robust electrical properties suggest CuO nanowires as promising candidates for NEMS actuators. Full article

In order to study the effects of kink-like defects in twin boundaries on deformation mechanisms and interaction between dislocations and defects in twin boundaries under localized load, nanotwinned Cu with two defective twin (TDT) boundaries is compared with the nanotwinned Cu with two perfect twin (TPT) boundaries, and nanotwinned Cu with single defective twin (SDT) boundary and single perfect twin boundary by simulating spherical nanoindentations using molecular mechanics. The indenter force-depth and hardness-contact strain responses were analyzed. Results show that the existence of intrinsic defects in twin boundary could reduce the critical load and critical hardness of nanotwinned material. A quantitative parameter was first proposed to evaluate the degree of surface atom accumulation around the indenter during nanoindentation, and it can be inferred that the surface morphology in TDT changes more frequently than the surface morphologies in TPT and SDT. The atomistic configurations of incipient plastic structures of three different models were also analyzed. We found that the intrinsic defects in twin boundary will affect the incipient plastic structures. The formation of twinning partial slip on the defective twin boundary happens before the contact of the dislocation and twin boundary. The kink-like defects could introduce Frank partial dislocation to the twin boundary during interaction between dislocation and twin boundary, which was not detected on the perfect twin boundary. In addition, the area of twinning partial slips on the upper twin boundary in the incipient plastic structures in SDT and TDT are larger than the twinning partial slip area in TPT, which results in the reduction of the critical hardness in SDT and TDT. The kink-like defects could also block the expansion of twinning partial slip on the twin boundary. Furthermore, we investigated the dislocation transmission processes in three different models. It is found that the dislocation transmission event could be delayed in model containing single defective twin boundary, while the transmission process could be advanced in model containing two consecutive defective twin boundaries. The quantitative analysis of dislocation length was also implemented. Result shows that the main emitted dislocation during nanoindentation is Shockley partial, and the dislocation nucleation in SDT and TDT is earlier than the dislocation nucleation in TPT due to the existence of defects. It is inferred that the intrinsic defects on twin boundaries could enhance the interaction between dislocations and twin boundaries, and could strongly change the structure evolution and promote the dislocation nucleation and emission. These findings about kink-like defects in twin boundaries show that the inherent kink-like defects play a crucial role in the deformation mechanisms and it should be taken into consideration in future investigations. Single defective twin boundary structure is recommended to delay the transmission and block the expansion of twin boundary migration. Some of the results are in good agreement with experiments. Full article

Molybdenum disulfide quantum dots (MoS₂ QDs) are a promising lubricant additive for enhanced engine efficiency. In this study, MoS₂ QDs were used as lubricating oil additives for ball-on-disc contact and had adequate dispersity in paroline oil, due to their super small particle size (~3 nm). Tribological results indicate that the friction coefficient of paroline oil with 0.3 wt.% MoS₂ QDs reached 0.061, much lower than that of pure paroline oil (0.169), which is due to the formation of a stable tribo-film formed by the MoS₂, MoO₃, FeS, and FeSO₄ composite within the wear track. Synergistic lubrication effects of the tribo-film and ball-bearing effect cooperatively resulted in the lowest friction and wear. Full article

The paper presents a statistical study of nanoindentation results obtained in seven European laboratories that have joined a round robin exercise to assess methods for the evaluation of indentation size effects. The study focuses on the characterization of ferritic/martensitic steels T91 and Eurofer97, envisaged as structural materials for nuclear fission and fusion applications, respectively. Depth-controlled single cycle measurements at various final indentation depths, force-controlled single cycle and force-controlled progressive multi-cycle measurements using Berkovich indenters at room temperature have been combined to calculate the indentation hardness and the elastic modulus as a function of depth applying the Oliver and Pharr method. Intra- and inter-laboratory variabilities have been evaluated. Elastic modulus corrections have been applied to the hardness data to compensate for materials related systematic errors, like pile-up behaviour, which is not accounted for by the Oliver and Pharr theory, and other sources of instrumental or methodological bias. The correction modifies the statistical hardness profiles and allows determining more reliable indentation size effects. Full article

We systematically studied nanoindentation size effect on creep deformation in a La-based metallic glassy film, including holding depth effect and indenter size effect. Creep displacement was mainly dependent on both holding strain and deformation volume beneath indenter. Under elastic holding, creep strain was merely holding strain–dependent. While for plastic holding, creep strain was greatly enhanced by adopting smaller indenter and/or decreasing holding depth at the same holding strain. A strong nanoindentation size effect on creep resistance was validated. Strain rate sensitivities (SRS) were calculated, which were obviously higher at elastic regions than at plastic holdings. The relationship between SRS value and creep mechanism in metallic glass was discussed. Full article

Surface mechanical properties of low-density polyethylene (LDPE) reinforced by carbon nanofibers (CNFs) up to 3% weight load were investigated using nanoindentation (NI). Surface preparation of the nanocomposite was thoroughly investigated and atomic force microscopy (AFM) was used to analyze the surface roughness of the polished surfaces. The dispersion of nanofillers in the LDPE matrix was examined using scanning electron microscopy (SEM). The effect of various penetration loads on the results and scattering of the data points was discussed. It was found by NI results that the addition of 3% weight CNF increased the elastic modulus of LDPE by 59% and its hardness up to 12%. The nano/micro-scale results were compared with macro-scale results obtained by the conventional tensile test as well as the theoretical results calculated by the Halpin-Tsai (HT) model. It was found that the modulus calculated by nanoindentation was twice that obtained by the conventional tensile test which was shown to be in excellent agreement with the HT model. Experimental results indicated that the addition of CNF to LDPE reduced its wear resistance property by reducing the hardness to modulus ratio. SEM micrographs of the semicrystalline microstructure of the CNF/LDPE nanocomposite along with the calculated NI imprints volume were examined to elaborate on how increasing the penetration depth resulted in a reduction of the coefficient of variation of the NI data/more statistically reliable data. Full article

Stress concentration around nanosized defects such as cavities always leads to plastic deformation and failure of solids. We investigate the effects of depth, size, and shape of a lotus-type nanocavity on onset plasticity of single crystal Al during nanoindentation on a (001) surface using a quasicontinuum method. The results show that the presence of a nanocavity can greatly affect the contact stiffness (S_c) and yield stress (σ_y) of the matrix during nanoindentation. For a circular cavity, the S_c and σ_y gradually increase with the cavity depth. A critical depth can be identified, over which the S_c and σ_y are insensitive to the cavity depth and it is firstly observed that the nucleated dislocations extend into the matrix and form a y-shaped structure. Moreover, the critical depth varies approximately linearly with the indenter size, regarding the same cavity. The S_c almost linearly decreases with the cavity diameter, while the σ_y is slightly affected. For an ellipsoidal cavity, the S_c and σ_y increase with the aspect ratio (AR), while they are less affected when the AR is over 1. Our results shed light in the mechanical behavior of metals with cavities and could also be helpful in designing porous materials and structures. Full article

Atomic force microscopy (AFM) has emerged as a popular tool for the mechanical mapping of soft nanomaterials due to its high spatial and force resolution. Its applications in rigid nanomaterials, however, have been underexplored. In this work, we studied elasticity mapping of common rigid materials by AFM, with a focus on factors that affect the accuracy of elasticity measurements. We demonstrated the advantages in speed and noise level by using high frequency mechanical mapping compared to the classical force volume mapping. We studied loading force dependency, and observed a consistent pattern on all materials, where measured elasticity increased with loading force before stabilizing. Tip radius was found to have a major impact on the accuracy of measured elasticity. The blunt tip with 200 nm radius measured elasticity with deviation from nominal values up to 13% in different materials, in contrast to 122% by the sharp tip with 40 nm radius. Plastic deformation is believed to be the major reason for this difference. Sharp tips, however, still hold advantages in resolution and imaging capability for nanomaterials. Full article