Scanning electron microscopy characteristics

Physical testing appHcations and methods for fibrous materials are reviewed in the Hterature (101—103) and are generally appHcable to polyester fibers. Microscopic analyses by optical or scanning electron microscopy are useful for evaluating fiber parameters including size, shape, uniformity, and surface characteristics. Computerized image analysis is often used to quantify and evaluate these parameters for quaUty control. 

To ensure quality control material suppliers and developers routinely measure such complex properties as molecular weight and its distribution, crystallinity and crystalline lattice geometry, and detailed fracture characteristics (Chapter 6). They use complex, specialized tests such as gel permeation chromatography (2, 3), wide- and narrow-angle X-ray diffraction, scanning electron microscopy, and high-temperature pressurized solvent reaction tests to develop new polymers and plastics applications. 

Scanning Electron Microscopy in the Study of Solid Propellant Combustion. Part 111. The Surface Structure and Profile Characteristics of Burning Composite Solid Propellants , NavWeps-Cent r TP 5142-Part 3 (1971) 48) B.T. 

Coacervation occurs in tropoelastin solutions and is a precursor event in the assembly of elastin nanofibrils [42]. This phenomenon is thought to be mainly due to the interaction between hydro-phobic domains of tropoelastin. In scanning electron microscopy (SEM) picmres, nanofibril stmc-tures are visible in coacervate solutions of elastin-based peptides [37,43]. Indeed, Wright et al. [44] describe the self-association characteristics of multidomain proteins containing near-identical peptide repeat motifs. They suggest that this form of self-assembly occurs via specific intermolecular association, based on the repetition of identical or near-identical amino acid sequences. This specificity is consistent with the principle that ordered molecular assembhes are usually more stable than disordered ones, and with the idea that native-like interactions may be generally more favorable than nonnative ones in protein aggregates. 

This technique can be applied to samples prepared for study by scanning electron microscopy (SEM). When subject to impact by electrons, atoms emit characteristic X-ray line spectra, which are almost completely independent of the physical or chemical state of the specimen (Reed, 1973). To analyse samples, they are prepared as required for SEM, that is they are mounted on an appropriate holder, sputter coated to provide an electrically conductive surface, generally using gold, and then examined under high vacuum. The electron beam is focussed to impinge upon a selected spot on the surface of the specimen and the resulting X-ray spectrum is analysed. 

Because of the instrumental requirements, these are usually not routine monitoring techniques. However, unlike other methods, they give detailed information on particle shapes. In addition, chemical composition information can be obtained using transmission electron microscopy (TEM) or scanning electron microscopy (SEM) combined with energy-dispersive spectrometry (EDS). The electron beam causes the sample to emit fluorescent X-rays that have energies characteristic of the elements in the sample. Thus a map showing the distribution of elements in the sample can be produced as the electron beam scans the sample. 

X-ray fluorescence (XRF). The sample is irradiated with monochromatic X-rays that eject electrons from the inner shells of the elements. When an electron from an outer shell of the ion drops into the vacancy, it emits characteristic X-rays whose wavelength is used to identify the element and whose intensity is related to the amount present. XRF is used primarily for elements heavier than magnesium because of the weak fluorescence of lighter elements and absorption of the X-rays within the particles. The combination of transmission or scanning electron microscopy (TEM/SEM) with X-ray fluorescence, also known as energy-dispersive spectrometry (EDS), was discussed in Section B.2b. 

Data collected for each run included acid analysis using inductively coupled plasma (ICF) to determine cation concentration and titration to determine H concentration. Filtering characteristics were determined using solid and filtrate yield rates, as well as back pressures during the filtration cycle. The filter cake was characterized by moisture content and composition. Solid samples were analyzed with scanning electron microscopy (SEM) to determine changes in particle shape and size under various process conditions, and X-ray diffraction (XRD) was used to determine the solids composition. 

Transmission electron microscopy (TEM) has traditionally been the mainstay of morphological investigations of polyolefins [8], but recent developments in low voltage high-resolution field emission gun scanning electron microscopy (FEG-SEM) [9] and the advent of atomic force microscopy (AFM) and related near-field techniques [10] have challenged its dominance at the length scales of the order of 10 nm, characteristic of both microdeformation (cavitation, fibrils) and structural components of semicrystalline... 

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