ABSTRACT
Cryogenic electron microscopy (cryo-EM) is a powerful tool for imaging liquid and semiliquid systems. While cryogenic transmission electron microscopy (cryo-TEM) is a standard technique in many fields, cryogenic scanning electron microscopy (cryo-SEM) is still not that widely used and is far less developed. The vast majority of systems under investigation by cryo-EM involve either water or organic components. In this paper, we introduce the use of novel cryo-TEM and cryo-SEM specimen preparation and imaging methodologies, suitable for highly acidic and very reactive systems. Both preserve the native nanostructure in the system, while not harming the expensive equipment or the user. We present examples of direct imaging of single-walled, multiwalled carbon nanotubes and graphene, dissolved in chlorosulfonic acid and oleum. Moreover, we demonstrate the ability of these new cryo-TEM and cryo-SEM methodologies to follow phase transitions in carbon nanotube (CNT)/superacid systems, starting from dilute solutions up to the concentrated nematic liquid-crystalline CNT phases, used as the 'dope' for all-carbon-fibre spinning. Originally developed for direct imaging of CNTs and graphene dissolution and self-assembly in superacids, these methodologies can be implemented for a variety of highly acidic systems, paving a way for a new field of nonaqueous cryogenic electron microscopy.
ABSTRACT
Acid spun carbon nanotube (CNT) fibers were investigated for their field emission properties and performance was determined to be dependent on fiber morphology. The fibers were fabricated by wet-spinning of pre-made CNTs. Fiber morphology was controlled by a fabrication method and processing conditions, as well as purity, size, and type of the CNT starting material. The internal fiber structure consisted of CNT fibrils held together by van der Waals forces. Alignment and packing density of the CNTs affects the fiber's electrical and thermal conductivity. Fibers with similar diameters and differing morphology were compared, and those composed of the most densely packed and well aligned CNTs were the best field emitters as exhibited by a lower turn-on voltage and a larger field enhancement factor. Fibers with higher electrical and thermal conductivity demonstrated higher maximum current before failure and longer lifetimes. A stable emission current at 3 mA was obtained for 10 h at a field strength of <1 V µm(-1). This stable high current operation makes these CNT fibers excellent candidates for use as low voltage electron sources for vacuum electronic devices.
