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Accurate extraction of liquid is the first step towards low-volume liquid delivery and nanocharacterization, which plays a significant role in biomedical research. In this study, a tip-shaped graphene nanopipette (GNP) is proposed by encapsulating the biomolecule solution on the prefabricated metal tip with graphene. The volume of the encapsulated liquid is highly controllable at zeptoliter precision by tuning the encapsulating speed and the number of graphene encapsulation rounds. Using protein (ferritin) solution as an example, it has been confirmed by finite element analysis and the controlled experiments that the GNP allows the delivery of ferritin solution at the zeptoliter-scale. Furthermore, GNP is demonstrated as a new type of tip-shaped liquid cell, which is suitable for multiple nanocharacterization techniques. In particular, due to the ultra-sharp tip shape, isotope (13C)-labelled glucose solution encapsulated in GNP has been characterized by atom probe tomography (APT) in the laser-pulsed mode. Analysis of the mass spectrum and the reconstructed three-dimensional chemical maps reveals the quantitative distribution and the compositions of individual glucose molecules. The GNP is expected to be introduced to deliver liquid in the range of zeptoliters to attoliters, and brings a new capability for characterization of biological specimens in their near-native state.

The evolution of atomistic-level nanostructure during the early stages of both standard, high-temperature T6 heat treatment, and low-temperature secondary ageing after interruption of the former (T6I4), has been investigated in rapid hardening Al-Cu-Mg alloys using a variety of microscopy and microanalytical techniques, including transmission electron microscopy (TEM), positron annihilation spectroscopy (PAS) and atom probe tomography (APT). In order to carry out this objective, quantitative data-analysis methods were developed with respect to new cluster-finding algorithms, specifically designed for use with three-dimensional APT data. Prior to this detailed characterisation work, the actual thermal impact from both heat treatment and quenching of small, lab-scale specimens was determined through correlation of both experimental results and calculations that modelled the heat transfer conditions using the lumped capacitance method. Subsequently, the maximum diffusion distance by random walk of the solute atoms was calculated for these periods, bearing significance on the propensity for these atoms to have the ability to cluster together, rather than segregate to the dislocation loops in the microstructure, which have a relatively larger interspacing distance. Age-hardening curves for the Al-1.1Cu-xMg (x = 0, 0.2, 0.5, 0.75, 1.0, 1.7 at.%) alloys at 150ºC show that the rapid hardening phenomenon (RHP) exists for Mg compositions ≥ 0.5Mg. Given that zone-like precipitate structures were unable to be detected by TEM or APT during the early stages of ageing at 150ºC, and that statistically significant dispersions of clusters were found in the APT data after ageing for 60 s, the RHP is attributed to these clustering reactions. Identification of clusters in the APT data has been achieved using the core-linkage algorithm and they have been found to be quite small, containing only a few atoms up to a couple of tens of atoms. The RHP is governed by some critical number density of both Mg clusters and Cu-Mg co-clusters of a critical size, whereas Cu clusters do not contribute significantly to the hardening mechanism. Significance testing indicates that Mg clusters are more significant at smaller clusters sizes and Cu-Mg co-clusters more important at larger cluster sizes. Hardness results also confirm the existence of rapid early hardening during secondary ageing at 65ºC in Al-1.1Cu-1.7Mg. The mechanism of secondary rapid hardening involves a combination of both secondary clustering from solute (mainly Mg atoms) residual in solution, and pre-existing amorphous primary clusters that have slower growth kinetics at the lower secondary ageing temperature. The latter occurs mainly by vacancy-assisted diffusion of Mg atoms as evidenced by the gradual increase of the Mg:Cu ratio of co-clusters. From an alloy design point of view it is important to fully understand the solute distribution in the microstructure to be able to subsequently optimise the configuration for enhanced material properties. The change in dispersion of solute atoms during ageing was determined by combining calculations of % vacancy-solute associations with detailed measurements of the dislocation loops to estimate the solute distribution within the microstructure. The implication of the balance of solute atoms segregated to the loops compared with that in the matrix is then discussed in the context of hardnening mechanisms.

The effect of Mo on the clustering and interphase precipitation occurring during phase transformation has been investigated in a strip-cast low-carbon steel containing Nb. In this work, isothermal coiling treatments were performed at 700 °C for various times to form interphase precipitates. Transmission electron microscopy (TEM), small-angle neutron scattering (SANS) and atom probe tomography (APT) results show that the addition of Mo increases the number density and volume fraction of clusters and interphase precipitates but has a negligible effect on their size, and overall provides for greater strengthening in the Mo-containing alloy. APT analysis shows that the interphase precipitates are composed of Nb, C and N in both alloys. The segregation of Mo is also observed in the interphase precipitates in the Mo-containing alloy, which is believed to relieve the lattice misfit between the precipitate and the matrix. It is proposed that the reduced lattice misfit allows for precipitate nucleation to occur more easily in the Mo-containing alloy Refereed/Peer-reviewed

Two low-C steels microalloyed with niobium (Nb) were fabricated by simulated strip casting, one with molybdenum (Mo) and the other without Mo. Both steels were heat treated to simulate coiling at 900 &deg, C to investigate the effect of Mo on the precipitation behaviour in austenite in low-C strip-cast Nb steels. The mechanical properties results show that during the isothermal holding at 900 &deg, C the hardness of both steels increases and reaches a peak after 3000 s and then decreased after 10,000 s. Additionally, the hardness of the Mo-containing steel is higher than that of the Mo-free steel in all heat-treated conditions. Thermo-Calc predictions suggest that MC-type carbides exist in equilibrium at 900 &deg, C, which are confirmed by transmission electron microscopy (TEM). TEM examination shows that precipitates are formed after 1000 s of isothermal holding in both steels and the size of the particles is refined by the addition of Mo. Energy dispersive spectroscopy (EDS) and electron energy loss spectroscopy (EELS) reveal that the carbides are enriched in Nb and N. The presence of Mo is also observed in the particles in the Nb-Mo steel during isothermal holding at 900 &deg, C. The concentration of Mo in the precipitates decreases with increasing particle size and isothermal holding time. The precipitates in the Nb-Mo steel provide significant strengthening increments of up to 140 MPa, higher than that in the Nb steel, ~96 MPa. A thermodynamic rationale is given, which explains that the enrichment of Mo in the precipitates reduces the interfacial energy between precipitates and matrix. This is likely to lower the energy barrier for their nucleation and also reduce the coarsening rate, thus leading to finer precipitates during isothermal holding at 900 &deg, C.

Molybdenum (Mo) is known to have a complex effect on phase transformations and precipitation in steels manufactured by conventional casting. The present work aims to examine the effect of Mo on phase transformations in Nb-containing steels produced by strip casting. Advanced experimental techniques have been utilised to simulate the strip casting process, and the microstructural features of the rapid solidification are retained for further study. Two cooling conditions from the austenite phase field were examined, isothermal holding and continuous cooling. It was found that at high cooling rates, the addition of Mo delayed the nucleation of bainite and lowered the bainite start temperature, but did not alter the bainite growth rate. The addition of Mo was also found to result in a slower transformation rate of polygonal ferrite under both isothermal and continuous cooling conditions. Thermodynamic simulations indicated that Mo did not affect the growth velocity of the polygonal ferrite, and quantitative metallography showed the nucleation density was significantly reduced by Mo addition. For the slowest continuous cooling rate, the addition of Mo completely inhibited pearlite formation, with bainitic ferrite forming instead. This has been suggested to be the result of the suppression of pearlite nucleation, rather than inhibition of growth. Refereed/Peer-reviewed

As-cast low-carbon low-niobium steels fabricated by direct strip casting (DSC) were treated by simulated coiling in the lab. Coiling temperatures were carefully selected: (1) 900 °C (in the austenite); (2) 700 °C (during the austenite-to-ferrite transformation); (3) 650 °C (in the ferrite). Optical microscopy and transmission electron microscopy were used to examine the microstructure constituents and the precipitates. Mechanical properties were evaluated by Vickers macrohardness measurements. The results show that coiling treatment has a strong influence on the final microstructure and mechanical properties, thus highlighting the necessity to carefully design the coiling treatment. In addition, the differences in hardness for the three coiling temperatures derive from a complex combination of different strengthening mechanisms. Refereed/Peer-reviewed

The use of rapid solidification processes such as direct strip casting (DSC) is a good way to refine the Fe-intermetallics and decrease their detrimental effects. DSC creates out-ofequilibrium supersaturated microstructures. In this work, we explore the precipitation phenomena in direct strip cast Al-Fe and Al-Cu-Fe alloys and related corrosion and mechanical properties. The precipitates are characterised with differential scanning calorimetry and transmission electron microscopy. The corrosion performances are evaluated with immersion tests and weight loss measurements and the yield strength and ductility are estimated with tensile tests. A strong correlation between the microstructure and the bulk properties is revealed with a significant improvement of properties of DSC alloys.

During the strip casting of steels, solidification occurs in a matter of milliseconds, and complete cooling to room temperature is complete in under 1 minute. Consequently, many steel alloys are meta-stable when processed by this method. These super-saturated alloys show unusual nano-scale behaviours such as room temperature clustering, nano-precipitation, and exhibit rather complex phase transformation characteristics during austenite decomposition. This presentation will demonstrate how advanced characterisation techniques such as atom probe tomography and small-angle neutron scattering have enabled better understanding of these phenomena.