Short-Time Magnetron Sputtering for the Development of Carbon-Palladium Nanocomposites.

In recent nanomaterials research, combining nanoporous carbons with metallic nanoparticles, like palladium (Pd), has emerged as a focus due to their potential in energy, environmental and biomedical fields. This study presents a novel approach for synthesizing Pd-decorated carbons using magnetron sputter deposition. This method allows for the functionalization of nanoporous carbon surfaces with Pd nano-sized islands, creating metal-carbon nanocomposites through brief deposition times of up to 15 s. The present research utilized direct current magnetron sputtering to deposit Pd islands on a flexible activated carbon cloth substrate. The surface chemistry, microstructure, morphology and pore structure were analyzed using a variety of material characterization techniques, including X-ray photoelectron spectroscopy, X-ray diffraction, Raman spectroscopy, gas sorption analysis and scanning electron microscopy. The results showed Pd islands of varying sizes distributed across the cloth's carbon fibers, achieving high-purity surface modifications without the use of chemicals. The synthesis method preserves the nanoporous structure of the carbon cloth substrate while adding functional Pd islands, which could be potentially useful in emerging fields like hydrogen storage, fuel cells and biosensors. This approach demonstrates the possibility of creating high-quality metal-carbon composites using a simple, clean and economical method, expanding the possibilities for future nanomaterial-based applications.

Coupled Broad Ion Beam-Scanning Electron Microscopy (BIB-SEM) for polishing and three dimensional (3D) serial section tomography (SST).

Here we describe the first automated fully integrated in-microscope broad ion beam (BIB) system. Ar+-BIB has several advantages over Ga+ focused ion beam (FIB) and Xe+ plasma-FIB (PFIB) methods inducing less beam damage, especially for ion beam sensitive materials. It can mill areas several orders of magnitude larger (up to millimetre scale), and is not confined to the edge of the sample with associated curtaining issues. BIB is shown to have sputter rates up to five times higher than comparable FIB techniques. This new coupled BIB-SEM system (commercial name 'iPrep™II') enables in-microscope surface polishing to remove contaminants or damage for two dimensional (2D) imaging, as well as automated serial section tomography (SST) by milling and imaging hundreds of slices, cost and time efficiently. The milled slice thickness can be controlled from a few nanometers up to a micrometre. A novel sample transfer, handling and interlock system allows automated and sequential BIB polishing, scanning electron microscopy (SEM) and analysis by secondary electron (SE) imaging, electron back scatter diffraction (EBSD) and energy dispersive spectroscopy (EDS) for 3D microstructure analysis. Furthermore, insulating surfaces can be sputter coated after milling each slice to reduce charging during SEM analysis. The performance of the instrument is demonstrated through a series of case studies across the materials, earth and life sciences exploiting the imaging, crystallographic and chemical mapping capabilities. These include the study of butterfly defects in bearing steels, meta-stable intermetallic phases in bronze bearings, shale gas rock, aluminium plasma electrolytic oxide (PEO) coatings as well as liver and mouse brain tissues.

3D Imaging of Indentation Damage in Bone.

Bone is a complex material comprising high stiffness, but brittle, crystalline bio-apatite combined with compliant, but tough, collagen fibres. It can accommodate significant deformation, and the bone microstructure inhibits crack propagation such that micro-cracks can be quickly repaired. Catastrophic failure (bone fracture) is a major cause of morbidity, particularly in aging populations, either through a succession of small fractures or because a traumatic event is sufficiently large to overcome the individual crack blunting/shielding mechanisms. Indentation methods provide a convenient way of characterising the mechanical properties of bone. It is important to be able to visualise the interactions between the bone microstructure and the damage events in three dimensions (3D) to better understand the nature of the damage processes that occur in bone and the relevance of indentation tests in evaluating bone resilience and strength. For the first time, time-lapse laboratory X-ray computed tomography (CT) has been used to establish a time-evolving picture of bone deformation/plasticity and cracking. The sites of both crack initiation and termination as well as the interconnectivity of cracks and pores have been visualised and identified in 2D and 3D.