An investigation on oxidation/carburisation of 9Cr-1Mo steel heat exchanger tube in an AGR environment

9Cr-1Mo steels have been used extensively in the power generation industry. In this study, a wide range of experimental samples exposed at different times and temperatures in a CO2 environment were analysed to look at the development of the metal and oxides over time. The main objective of this work was to obtain a better understanding of the carburisation and oxidation behaviour of 9Cr 1Mo steels as a function of temperature/time, with special attention paid to the transition from protective to breakaway oxidation. In addition, experiments were also carried out to investigate any links between oxidation transition and carburisation behaviour of these materials

In-situ micro bend testing of SiC and the effects of Ga+ ion damage

The Young’s modulus of 6H single crystal silicon carbide (SiC) was tested with micro cantilevers that had a range of cross-sectional dimensions with surfaces cleaned under different accelerating voltages of Ga+ beam. A clear size effect is seen with Young’s modulus decreasing as the cross-sectional area reduces. One of the possible reasons for such size effect is the Ga+ induced damage on all surfaces of the cantilever. Transmission electron microscopy (TEM) was used to analyse the degree of damage, and the measurements of damage is compared to predictions by SRIM irradiation simulation

Experimental studies of shear bands in Zr-Cu metallic glass

Shear bands are the key feature that controls deformation in bulk metallic glasses (BMGs). This study provides a comprehensive analysis of plastic deformation of a Zr-Cu-based BMG at room temperature. Experiments were conducted to observe the evolution of shear bands in the material. It was shown that shear bands formed discretely in the material which allows for material deformation to occur across it. Additionally, individual shear bands were characterised to obtain a better understanding of shear-band-induced plasticity. Assessment of mechanical properties, such as hardness and elastic modulus, indicate the deformed regions of the material were weaker than undeformed regions. No compositional or structural changes were found in shear-band of the studied BMG suggesting generation of local free volume in the deformed region

Focused ion beam preparation of microbeams for in situ mechanical analysis of electroplated nanotwinned copper with probe type indenters

A site‐specific xenon plasma focused ion beam preparation technique for microcantilever samples (1 μm ‐ 20 μm width and 1:10 aspect ratio) is presented. The novelty of the methodology is the use of a chunk lift‐out onto a clean silicon wafer to facilitate easy access of a low‐cost probe type indenter which provides bending force measurement. The lift‐out method allows sufficient room for the indenter and a line of sight for the electron beam to enable displacement measurement. An electroplated nanotwinned copper (NTC) was cut to a 3 × 3 × 25 μm micro‐beam and in‐situ mechanically tested using the developed technique. It demonstrated measured values of Youngs modulus of 78.7 ± 11 GPa and flow stress of 0.80 ± 0.05 GPa, which is within the ranges reported in the literature

Liquid – liquid phase separation morphologies in ultra-white beetle scales and a synthetic equivalent

Cyphochilus beetle scales are amongst the brightest structural whites in nature, being highly opacifying whilst extremely thin. However, the formation mechanism for the voided intra- scale structure is unknown. Here we report 3D x-ray nanotomography data for the voided chitin networks of intact white scales of Cyphochilus and Lepidiota stigma. Chitin-filling frac- tions are found to be 31 ± 2% for Cyphochilus and 34 ± 1% for Lepidiota stigma, indicating previous measurements overestimated their density. Optical simulations using finite- difference time domain for the chitin morphologies and simulated Cahn-Hilliard spinodal structures show excellent agreement. Reflectance curves spanning filling fraction of 5-95% for simulated spinodal structures, pinpoint optimal whiteness for 25% chitin filling. We make a simulacrum from a polymer undergoing a strong solvent quench, resulting in highly reflective ( 94%) white films. In-situ X-ray scattering confirms the nanostructure is formed through spinodal decomposition phase separation. We conclude that the ultra-white beetle scale nanostructure is made via liquid–liquid phase separation

Detection and quantification of precipitates in 11–12 wt% Cr steels using in-column secondary electron detectors

In order to quantify precipitates such as Laves phase, M23C6 carbides and modified Z-phase in 9 – 12 wt. % Cr power plant steels, a range of microscopy techniques, including scanning electron microscope (SEM) and focussed ion beam (FIB) imaging, are currently used. This paper’s key finding reports on the novel application of a field emission SEM (FESEM) in-column upper secondary electron detector (USD) for imaging and quantification of precipitates in a thermally aged 11 - 12 wt. % Cr steel sample. The USD produces images from first order secondary electrons generated directly from primary electron beam interaction. These images were found to not only show significant contrast between the matrix and the precipitates to enable quantification, but between particles which otherwise have identical greyscale intensities in FIB images. Previously assumed to be the same phase, some of these precipitates appeared significantly darker than others. The greyscale differential between these precipitate types was sufficient for separate quantification. Energy dispersive x-ray spectroscopy and selected area diffraction analysis identified the darker particles as modified Z-phase and the lighter grey particles as M23C6 carbides. When analysing all particles together, comparison of data from FESEM USD and FIB images confirmed that both techniques produce statistically comparable precipitate analysis results. However, as modified Z-phase and M23C6 carbide distributions can be analysed separately from a FESEM in-column USD image at low accelerating voltages, it was found that this technique provides for more reliable precipitate quantification than FIB imaging alone in these steels. With future work, this could enable faster characterisation and may lead to automated larger area mapping

Droplet factories: Synthesis and assembly of metal nanoparticles on magnetic supports

The interface between two immiscible liquids represent an ideal substrate for the assembly of nanomaterials. The defect free surface provides a reproducible support for creating densely packed ordered materials. Here a droplet flow reactor is presented for the synthesis and/or assembly of nanomaterials at the interface of the emulsion. Each droplet acts as a microreactor for a reaction between decamethylferrocene (DmFc) within the hexane and metal salts (Ag+/Pd2+) in the aqueous phase. The hypothesis was that a spontaneous, interfacial reaction would lead to the assembly of nanomaterials creating a Pickering emulsion. The subsequent removal of the solvents showed how the Ag nanoparticles remain trapped at the interface and retain the shape of the droplet, however the Pd nanoparticles were dispersed with no tertiary structure. To further exploit this, a one-step process where the particles are synthesised and then assembled into core-shell materials was proposed. The same reactions were performed in the presence of oleic acid stabilised iron oxide nanoparticles dispersed within the hexane. It was shown that by changing the reaction rate and ratio between metal and iron oxide a continuous coating of metal nanoparticles can be formed on top of an iron oxide microsphere, or form a uniform composite. These insights offer a new method and chemistry within flow reactors for the creation of palladium and silver nanoparticles. We use the technique to create metal coated iron oxide nanomaterials but the methodology could be easily transferred to the assembly of other materials

Raw Data used in "Detection and Quantification of Precipitates in 11 - 12 wt. % Cr Steels using In-Column Secondary Electron Detectors".xlsx

Raw data for the publication, "Detection and Quantification of Precipitates in 11 - 12 wt. % Cr Steels using In-Column Secondary Electron Detectors". </i