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We have measured the magnetic susceptibility and heat capacity of CuO nanoparticles (16 nm) from 2 K to 400 K using a Quantum Design Physical Properties Measurement System (PPMS). The magnetization curves, acquired at various field strengths from 0 Oe to 50 kOe, are similar to literature data of bulk and nanoscale CuO showing a minimum at about 150 K, an upturn as temperature approaches 0 K, and a broad maximum at high temperatures extending beyond 400 K. The heat capacity data between 200 K and 400 K show several broad peaks. The number of these peaks and the temperatures at which they occur differ significantly from the magnetic transitions known to exist in bulk CuO. To further investigate these transitions in nanoscale CuO, we performed temperature dependent x-ray diffraction (XRD) at temperatures from 90 K to 700 K from which lattice parameters as a function of temperature were derived using a Rietveld refinement. Although no phase transitions were observed in these data, changes in the slopes of the lattice parameters are apparent at the transition temperatures observed in the heat capacity and susceptibility measurements. The various transitions in the heat capacity data are attributed to competing ferromagnetic and antiferromagnetic interactions caused by structural properties that are unique to nanophase CuO, and the temperature range of multiferroicity in nanoscale CuO is shown to extend to temperatures higher than those observed for bulk CuO. The heat capacity and temperature dependent XRD measurements are the first of their kind to be reported for CuO nanoparticles.

The thermodynamic properties of hydrated α-Fe2O3 (hematite) and Fe3O4 (magnetite) nanoparticles have been comprehensively assessed. In addition to 9 nm Fe3O4, three α-Fe2O3 nanoparticles samples of different sizes (11, 14, and 25 nm) and bulk α-Fe2O3 have been evaluated by inelastic neutron scattering methods. The contribution of the two-level magnetic spin flip transition to the heat capacity of the α-Fe2O3 particles has been determined. The isochoric heat capacity of the water confined on the surface of these two types of iron oxide particles have been calculated from their INS spectra, and is affected by the chemical composition of the underlying particle. Furthermore, the heat capacity and dynamics of the particle hydration layers appear to be influenced by a complex array of factors including particle size, water coverage, and possibly the magnetic state of the particle itself.

The important variables in the synthesis of stable, high surface area, aluminum-modified anatase TiO2 catalyst supports were identified and optimized using statistically designed experiments (DOEs). The first DOE examined ten variables at two levels and a second DOE studied eight variables at three levels. Equations were developed to predict the conditions to obtain the highest surface area and pore volume at the desired pore diameter and predict the pore diameter range that may be obtained. Confirmation trials closely matched predicted surface areas, pore volumes, and pore diameters in all but one trial. Rinsing order (before or after calcination) was the most significant factor. Other important factors were calcination temperature, mol% aluminum, and water addition speed. The results of this study demonstrate (a) the power of DOEs in identifying and controlling synthesis variables in relatively few experiments and (b) how analysis of factor effects can provide insight into the formation mechanism.

Traditional Screening Designs, such as resolution III 2k-p fractional factorials are used routinely in the initial stages of process development. These designs are used to determine which process variables have the largest effect on process outcomes. Once a screening design is complete and the data are analysed, follow-up experiments are normally required in order to develop useful prediction equations involving the important variables and to identify the optimal process operating conditions. Recently developed definitive screening designs allow researchers to identify important variables and optimum process conditions after one set of experiments, eliminating the need for follow-up experiments. This leads to the question: What is now the role of traditional and definitive screening designs in process optimisation? We share our insights gained from using both of these designs in developing a process to produce catalyst support material to shed light on these questions.

Most of us heard the story of the blind men and the elephant as children. In this old tale from India each man in a group of blind men touches a different part of an elephant. Each walks away with a different experience and subsequently argues that the elephant is like a spear (the tusk), a rope (the tail), a wall (the flank), etc. Only the combination of their stories would have provided a complete, or at least more complete, picture of what an elephant really is.

The effects of iron catalyst thickness on the fabrication and performance of microfabricated, binder-free, carbon nanotube (CNT)-templated, thin layer chromatography (TLC) plates are demonstrated. The iron catalyst was deposited at thicknesses ranging from 4 to 18 nm in increments of 2 nm. Its thickness plays a key role in governing the integrity and separation capabilities of microfabricated TLC plates, as determined using a test dye mixture. Atomic force microscopy and scanning electron microscopy show that smaller and more numerous catalyst nanoparticles are formed from thinner Fe layers, which in turn govern the diameters and densities of the CNTs. The average diameter of the Fe nanoparticles, Dp, is approximately six times the initial Fe film thickness, tFe: Dp ≈ 6tFe. After deposition of relatively thick silicon layers on CNTs made with different Fe thicknesses, followed by oxidation, all of the resulting CNT-templated SiO2 wires had nearly the same diameter. Consequently, their surface areas were v...