Soot Morphology: An Application of Image Analysis in High Resolution Transmission Electron Microscopy

"Interest in the fine structure of soots and carbon blacks is motivated by a variety of possible applications. The structure provides information on the origins of the particles and on their adsorptive and reactive properties. This paper describes a method for quantification of the structure of soots and carbon blacks based on direct electron microscopic observation followed by image analysis of these materials. High-resolution transmission electron microscopy (HRTEM) provides a very detailed observation of particle structure. The differences in soot structure, because of its complexity, may not be easily quantifiable with the human eye; therefore, high-level computer software has been used to manipulate HRTEM images. This technique involves the application of fast Fourier transforms (FFT) to single particles and the measurement of characteristic parameters such as interplanar spacings and crystallite sizes from these particles. The methodology and application of this characterization technique are presented here. Results are shown for dif¬ferent samples obtained from soot and carbon black particles selected to illustrate the capabilities of the methodology. Quantitative information can be obtained on structural characteristics, e.g., interplanar spacing, circularity, orientation, elongation, and length distribution of lattice fringes, as well as on the fractional coverage of the extracted pattern. c 1996 Wiley-Liss, Inc.This paper presents a combination of techniques for recognizing and classifying different carbonaceous materials, using their structural morphology. A new method to assess and quantify the parameters which define such structures is proposed and discussed. The technique is based on the use of HRTEM (high-resolution transmission electron microscopy) and computational image analysis.It is well-known that carbonaceous materials like graphite, soots, coals, cokes, chars, etc. possess characteristic structural appearances which can vary from mostly random or amorphous to a perfectly ordered graphitic crystalline structure (Buseck and Bo-Jun, 1985; Buseck et al., 1987). The carbon structure has been variously described as turbostratic (Oberlin, 1989) or as crumpled sheets (Rouzaud et al., 1991) to indicate that parallel layering, reminiscent of graphite, is observed over dimensions of nanometers, but that these planes or crystallites show disorder over larger scales. The degree of order of such structures is strongly dependent on the thermal treatment of the material as well as on the composition of the source of the carbonaceous material. The value of the electron microscope in studying the morphology of such materials has been well-established, and abundant information is available (Ishiguro et al., 1991; Lahaye and Prado, 1978; Buseck, 1992).The use of HRTEM has brought further insight into this matter. Qualitative assessment of the structural order of such materials has been attempted over a long period of time in order to differentiate between various sources or treatments. There is, to date, no successful method available for quantifying the structural characteristics of various carbonaceous materials. This paper presents a technique which is able to recognize dif-ferent materials and to quantify the structural parameters of those materials using HRTEM and computational image analysis, including pattern recognition techniques.In the case of perfectly ordered graphitic crystals, electron diffraction is widely used for obtaining details on structure. Analysis of diffraction patterns can reveal parameters such as interplanar spacing, d002, crystallite size along the c-axis, Lc, crystal size in the plane of the layers, L., mean number of crystallites, Nc, etc.Complicated electron microscopy methods such as defocusing, tilted illumination, axial illumination, etc., often have to be used in order to characterize complex materials such as randomly oriented crystals in soots and carbons. Obtaining the right fo"