Nine halloysite nanotubes (HNTs) have been examined using scanning electron microscopy (SEM), atomic force microscopy (AFM) and (cross-sectional) transmission electron microscopy (TEM) to evaluate details of their external and internal morphologies. The samples span morphologies within the cylindrical to prismatic-polygonal framework proposed by Hillier et al. (2016). The ‘carpet roll’ model assumed in the conceptualization of most technological applications of HNTs is shown to be far too simplistic. Both cylindrical and prismatic forms have abundant edge steps traversing their surfaces that, by analogy with plates of kaolinite, correspond to prism faces. The mean value for the diameter of the central lumen of the tubes is 12 nm. Numerous slit-like nanopores, with diameters up to 18 nm, also occur between packets of layers, particularly in prismatic forms at the junction between a central cylindrical core and outer packets of planar layers. These pores expose aluminol and siloxane surfaces, but unlike the lumen, which is assumed only to expose an aluminol surface, they do not extend along the entire length of the nanotube. Edge steps seen most clearly by AFM correspond in height to the packets of layers seen in TEM. TEM cross-sections suggest that tube growth occurs by accretion of a spiralled thickening wedge of layers evolving from cylindrical to polygonal form and reveal that planar sectors may be joined by either abrupt angular junctions or by short sections of curved layers. A more realistic model of the internal and external morphologies of HNTs is proposed to assist with understanding of the behaviour of HNTs in technological applications.

Twenty one samples of relatively pure tubular halloysites (HNTs) from localities in Australia, China, New Zealand, Scotland, Turkey and the USA have been investigated by X-ray diffraction (XRD), infrared spectroscopy (IR) and electron microscopy. The halloysites occur in cylindrical tubular forms with circular or elliptical cross sections and curved layers and also as prismatic tubular forms with polygonal cross sections and flat faces. Measurements of particle size indicate a range from 40 to 12,700 nm for tube lengths and from 20 to 600 nm for diameters. Size distributions are positively skewed with mean lengths ranging from 170 to 950 nm and mean diameters from 50 to 160 nm. Cylindrical tubes are systematically smaller than prismatic ones. Features related to order/ disorder in XRD patterns e.g. as measured by a ‘cylindrical/prismatic’ (CP) index and IR spectra as measured by an ‘OH-stretching band ratio’ are related to the proportions of cylindrical vs. prismatic tubes and correlated with other physical measurements such as specific surface area and cation exchange capacity. The relationships of size to geometric form, along with evidence for the existence of the prismatic form in the hydrated state and the same 2M1 stacking sequence irrespective of hydration state (i.e. 10 vs. 7 Å) or form, suggests that prismatic halloysites are the result of continued growth of cylindrical forms.

Metallic silver nanoparticles were synthesized using a hydrothermal route for use in high throughput biosensing applications. Particle shape was engineered by varying polyvinyl pyrollidone (PVP) concentration in the precursor mixture, resulting in the emergence of flat triangular shaped nanoparticles with increasing PVP content. The hydrothermal method was found to yield particles with better particle size distribution and longer shelf life relative to polyol synthesis particles.

The templating of hydrolysed silane species by self-assembling peptide fibrils has been extensively studied at the Centre for Self Organising Molecular Systems based in the University of Leeds . In this paper we present an SEM based study of the pH effects on the peptide fibril templates and the fluoride catalysed templating chemistry and the resulting silica nanotubes.

Advanced analytical transmission electron microscopy has been used to investigate microstructural evolution during pyrolysis in triol-based sol-gel thin films. At pyrolysis temperatures up to 300 °C, the films remained amorphous; however, nanometer-sized precipitates were observed in films heat-treated up to 400 °C for 10 min. Analytical transmission electron microscopy indicated that the precipitates were Pb-rich, as well as deficient in O, Ti, and Zr. Films pyrolyzed up to 500 °C for 10 min were composed of a nanocrystalline pyrochlore phase; however, pores could be observed, situated in the same position as the nanometer-sized precipitates at 400 °C. Face-centered cubic Pb-rich crystallites were also present on the surface of pyrolyzed films but absent in the fully crystallized films annealed at 650 °C. A tentative mechanism is proposed to explain these observations.

Polycrystalline aluminas sintered with 10 wt% additions of calcium oxide (CaO) and silica (SiO2) in varying molar ratios were fabricated via precipitation, calcination, and hot pressing. Alumina microstructures were analyzed by scanning electron microscopy in terms of their mean grain size, grain size distribution, and grain aspect ratios. High-resolution transmission electron microscopy (HRTEM) showed the presence of an amorphous intergranular glassy phase at two- and three-grain boundaries. The intergranular film width at two-grain boundaries, determined by HRTEM, appeared to vary with the [CaO]:[SiO2] ratio of the additive as did the chemical composition and local chemistry, determined by high-resolution analytical transmission electron microscopy and scanning transmission electron microscopy (using both energy dispersive x-ray and electron energy loss spectroscopy). The factors influencing the erosive wear rate are discussed including the chemistry and associated fracture energy of the intergranular glassy film. Wet erosive wear rates of the densified materials were determined and had a strong dependence on the [CaO]:[SiO2] ratio in the additive.