An international round-robin calibration protocol for nanoindentation measurements

Nanoindentation has become a common technique for measuring the hardness and elastic-plastic properties of materials, including coatings and thin films. In recent years, different nanoindenter instruments have been commercialised and used for this purpose. Each instrument is equipped with its own analysis software for the derivation of the hardness and reduced Young's modulus from the raw data. These data are mostly analysed through the Oliver and Pharr method. In all cases, the calibration of compliance and area function is mandatory. The present work illustrates and describes a calibration procedure and an approach to raw data analysis carried out for six different nanoindentation instruments through several round-robin experiments. Three different indenters were used, Berkovich, cube corner, spherical, and three standardised reference samples were chosen, hard fused quartz, soft polycarbonate, and sapphire. It was clearly shown that the use of these common procedures consistently limited the hardness and reduced the Young's modulus data spread compared to the same measurements performed using instrument-specific procedures. The following recommendations for nanoindentation calibration must be followed: (a) use only sharp indenters, (b) set an upper cut-off value for the penetration depth below which measurements must be considered unreliable, (c) perform nanoindentation measurements with limited thermal drift, (d) ensure that the load-displacement curves are as smooth as possible, (e) perform stiffness measurements specific to each instrument/indenter couple, (f) use Fq and Sa as calibration reference samples for stiffness and area function determination, (g) use a function, rather than a single value, for the stiffness and (h) adopt a unique protocol and software for raw data analysis in order to limit the data spread related to the instruments (i.e. the level of drift or noise, defects of a given probe) and to make the H and E r data intercomparable. © 2011 Elsevier Ltd.

Comparisons of the two-body abrasive wear behaviour of four different ferrous microstructures with similar hardness levels

The abrasive wear resistance of four distinct metallurgical steel microstructures - bainite, pearlite, martensite and tempered martensite, with similar hardness levels was investigated. A pin-on-disc tribometer was used to simulate the two-body abrasive condition (i.e. the metallic surface abrading against the silicon carbide abrasive particles) and evaluate the specific wear rate of the microstructures. Each microstructure had a unique response towards the abrasion behaviour and this was largely evident in the friction curve. However, the multi-phase microstructures (i.e. bainite and pearlite) demonstrated better abrasion resistance than the single-phase microstructures (i.e. martensite and tempered martensite). Abrasion induced microstructural changes at the deformed surfaces were studied using sub-surface and topographical techniques. The properties of these layers (i.e. surface profile measurements) determined the amount of material loss for each microstructure. These were directly linked to the single-wear track analysis that highlighted a marked difference in their mode of material removal. Ploughing and wedge formation modes were dominant in the case of bainite and pearlite microstructures, whereas the cutting mode could be attributed to the higher material loss in the single-phase microstructures. The combination of brittle and ductile phases in the multi-phase microstructure matrix could be one of the driving factors for their superior abrasion resistance.

Microstructure and hardness evolution during simulated coiling of a direct strip cast low carbon low niobium steel

This paper examines the impact of coiling temperature and duration on the phase transformation and precipitation behavior of a low carbon and low niobium direct strip cast steel. Coiling was performed at three carefully chosen temperatures: (1) in the ferrite (600°C), (2) during the austenite decomposition (700°C) and (3) in the austenite (850°C). The coiling conditions were found to strongly affect the final microstructure and hardness response, thus highlighting the necessity to judiciously design the coiling treatment. Optical microscopy, and scanning and transmission electron microscopy were used to characterize the microstructural constituents (polygonal ferrite, bainite and pearlite) and the NbC precipitates. Vickers macrohardness measurements are utilized to quantify the mechanical properties. The differences in hardening kinetics for the three different temperatures are shown to come from a complex combination of strengthening contributions.

Quantification of motor vehicle emission factors from on road measurements

Assessment and prediction of the impact of vehicular traffic emissions on air quality and exposure levels requires knowledge of vehicle emission factors. The aim of this study was quantification of emission factors from an on road, over twelve months measurement program conducted at two sites in Brisbane: 1) freeway type (free flowing traffic at about 100 km/h, fleet dominated by small passenger cars - Tora St); and 2) urban busy road with stop/start traffic mode, fleet comprising a significant fraction of heavy duty vehicles - Ipswich Rd. A physical model linking concentrations measured at the road for specific meteorological conditions with motor vehicle emission factors was applied for data analyses. The focus of the study was on submicrometer particles; however the measurements also included supermicrometer particles, PM2.5, carbon monoxide, sulfur dioxide, oxides of nitrogen. The results of the study are summarised in this paper. In particular, the emission factors for submicrometer particles were 6.08 x 1013 and 5.15 x 1013 particles per vehicle-1 km-1 for Tora St and Ipswich Rd respectively and for supermicrometer particles for Tora St, 1.48 x 109 particles per vehicle-1 km-1. Emission factors of diesel vehicles at both sites were about an order of magnitude higher than emissions from gasoline powered vehicles. For submicrometer particles and gasoline vehicles the emission factors were 6.08 x 1013 and 4.34 x 1013 particles per vehicle-1 km-1 for Tora St and Ipswich Rd, respectively, and for diesel vehicles were 5.35 x 1014 and 2.03 x 1014 particles per vehicle-1 km-1 for Tora St and Ipswich Rd, respectively. For supermicrometer particles at Tora St the emission factors were 2.59 x 109 and 1.53 x 1012 particles per vehicle-1 km-1, for gasoline and diesel vehicles, respectively.

Loading applied on prosthetic knee of transfemoral amputee: comparison of inverse dynamics and direct measurements

Inverse dynamics is the most comprehensive method that gives access to the net joint forces and moments during walking. However it is based on assumptions (i.e., rigid segments linked by ideal joints) and it is known to be sensitive to the input data (e.g., kinematic derivatives, positions of joint centres and centre of pressure, inertial parameters). Alternatively, transducers can be used to measure directly the load applied on the residuum of transfemoral amputees. So, the purpose of this study was to compare the forces and moments applied on a prosthetic knee measured directly with the ones calculated by three inverse dynamics computations - corresponding to 3 and 2 segments, and « ground reaction vector technique » - during the gait of one patient. The maximum RMSEs between the estimated and directly measured forces (i.e., 56 N) and moment (i.e., 5 N.m) were relatively small. However the dynamic outcomes of the prosthetic components (i.e., absorption of the foot, friction and limit stop of the knee) were only partially assessed with inverse dynamic methods.

Application of bag sampling technique for particle size distribution measurements

Bag sampling techniques can be used to temporarily store an aerosol and therefore provide sufficient time to utilize sensitive but slow instrumental techniques for recording detailed particle size distributions. Laboratory based assessment of the method were conducted to examine size dependant deposition loss coefficients for aerosols held in VelostatTM bags conforming to a horizontal cylindrical geometry. Deposition losses of NaCl particles in the range of 10 nm to 160 nm were analysed in relation to the bag size, storage time, and sampling flow rate. Results of this study suggest that the bag sampling method is most useful for moderately short sampling periods of about 5 minutes.