A tilting procedure to enhance compositional contrast and reduce residual diffraction contrast in energy-filtered TEM imaging of planar interfaces.

This paper systematically demonstrates that energy-filtered transmission electron microscope (EFTEM) images of a planar interface between two single crystals have increased compositional contrast and decreased residual diffraction contrast when the sample is oriented so that the electron beam is parallel to the interface, but not directly on a zone axis. This off-axis orientation reduces diffraction contrast in the unfiltered (and zero-loss) image, which in turn, reduces residual diffraction contrast in single energy-filtered TEM (EFTEM) images, thickness maps, jump-ratio images, and elemental maps. Most importantly, this procedure produces EFTEM images that are more directly interpretable and, in most cases, possess superior spatial resolution compared to EFTEM images acquired directly on a zone axis.

High-resolution and analytical transmission electron microscopy of mineral disorder and reactions.

Crystal defects and chemical reactions occurring at scales beyond the resolution of light microscopes have major effects on the chemical and physical properties of rocks and minerals. High-resolution imaging, diffraction, and chemical analysis in the transmission electron microscope have become important methods for exploring mineral defect structures and reaction mechanisms and for studying the distribution of phases resulting from reactions. These techniques have shown that structural disorder is common in some rock-forming minerals but rare in others. They have also established mechanisms by which many reactions occur at the atomic cluster scale. These data thus provide an atomistic basis for understanding the kinetics of geological reactions. Furthermore, apparent major-element, minor-element, and trace-element chemistry of minerals can be influenced by submicroscopic inclusions or intergrowths, which commonly form as products of solid-state reactions.

Exsolution of hornblende and the solubility limits of calicum in orthoamphibole.

Exsolution between orthorhombic and monoclinic amphibole has been postulated for many years on the basis of crystal-chemical and structural differences. Transmission and analytical electron microscope examination of calium-rich gedrite specimens from southwestern New Hampshire has now revealed evidence for exsolution of calcic clinoamphibole (hornblende) from ferromagnesian orthoamphibole. Analytical electron microscopy data suggests that calcium has a low solubility limit in the orthoamphibole structure. The hornblende lamellae range from only a few unit cells in thickness to about 80 nanometers. The formation of the calcic amphibole lamellae resulted from heterogeneous nucleation and growth along pre-existing (100) stacking faults. Thus, the deformation processes producing the stacking faults played a key role in preparing the sites for exsolution.

Potassium in clinopyroxene inclusions from diamonds.

Analytical transmission electron microscopy, electron microprobe analyses, and singlecrystal x-ray diffraction data support the conclusion that high potassium contents, up to 1.5 weight percent K(2)O, of some diopside and omphacite inclusions from diamonds represent valid clinopyroxene compositions with K in solid solution. This conclusion contradicts the traditional view of pyroxene crystal chemistry, which holds that K is too large to be incorporated in the pyroxene structure. These diopside and omphacite inclusions have a high degree of crystal perfection and anomalously large unit-cell volumes, and a defect-free structure is observed in K-bearing regions when imaged by transmission electron microscopy. These observations imply that clinopyroxene can be a significant host for K in the mantle and that some clinopyroxene inclusions and their diamond hosts may have grown in a highly K-enriched environment.

Serpentine minerals: intergrowths and new combination structures.

The serpentine minerals chrysotile, lizardite, and antigorite have been found intimately intergrown with each other and with talc, chlorite, and amphibole in incompletely reacted chain silicates. High-resolution transmission electron microscopy has revealed new variations in serpentine planar and roll structures, as well as regions of mixed-layer silicate consisting of serpentine and talc layers.

Asbestiform chain silicates: new minerals and structural groups.

The discovery and characterization of structurally ordered and disordered phases that are intermediate between amphiboles and micas have shown that the biopyriboles are a much more complex family of minerals than has previously been recognized. In addition to single-chain, double-chain, and sheet structures, there are also minerals with triple chains and with alternating double and triple chains. Many crystals exhibit disorder in the sequence of double and triple chains, and isolated chains that are wider than triple are common. This structural disorder helps to explain why asbestiform amphiboles are fibrous. The new phases have now been found in several localities, and it is possible that similar phenomena in other minerals could also have been overlooked. In particular, there is no reason to suppose that analogous substances and structures with both single and double chains do not occur between the pyroxenes and the amphiboles. Since the pyroxenes are used extensively by geologists to assess rock histories and formation temperatures and pressures, it is essential that the extent of this type of disorder be evaluated. It is possible that what appears to be only an interesting mineralogical problem may prove to be a petrological nightmare.