Abstract

Differences in lamellae length, stacking, and particularly a difference in the core-to-shell radial structure are observed for carbon blacks produced using different feedstocks. Carbon black (CB) produced using a coal tar (CT) feedstock formed particles with amorphous cores exhibiting a sharp transition to extended lamellae oriented about the periphery of the particle. In contrast, the carbon black produced from fluidized catalytic cracker (FCC) decant oil as feedstock formed particles with a single nucleated core possess a rather uniform radial transition—reflecting the presence of ordered, concentric lamellae across most of the particle radius. Minimal disorder was observed in the core while the undulations in perimeter lamellae were fewer. Our interpretation for these structural dissimilarities is premised on differences in fuel composition, specifically component classes as found by saturate, aromatic, resin, asphaltene (SARA) analysis. These in turn lead to variation in the relative rates of particle nucleation and particle growth by pyrolysis products, moderated by temperature. Electron energy loss spectroscopy reveals radial variation in the sp2 content between the different feedstocks consistent with observed nanostructures. Collectively these results are interpreted in terms of an offset in nucleation and growth—dependent upon the relative contributions of feedstock aromatic content and pyrolysis processes to particle nucleation and growth. To further test the postulate of different formation conditions for the two carbon blacks pulsed laser annealing was applied. The high temperature heating accentuated the dissimilarities in nanostructure and chemistry—leading to stark dissimilarities. These differences were also manifested by comparing oxidative reactivity.

Highlights

  • The energy loss measurements were taken using FEI Titan G2 microscope operated at 300 kV in scanning transmission electron microscopy (STEM) mode for high spatial resolution

  • While the degree of branching morphology appears to decrease with aggregate size, this is a consequence of the fewer primary particles within these aggregates but does not necessarily change the fractal descriptor

  • Lattice fringes, formed by the constructive interference of the transmitted and diffracted beams in a Transmission Electron Microscopy (TEM) provide a reconstruction of the lamellae structure and can be used to quantify the nanostructure of flame formed carbons or carbon black and differentiate between materials based on their lamellae arrangement

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Summary

Feedstocks

The two carbon blacks used in this study are derived from different feedstocks, described briefly as follows. Coal tar is an extremely complex mixture, containing 4, 5, 6, and even 7-ring aromatics, as well as methylated and poly-methylated derivatives with SARA analysis differentiating saturates and aromatic. SARA analysis results highlight the key differences relative to the CT material as higher saturate and lower aromatic content. FCC decant oils can contain an aromatic distribution ranging from single to 4-ring compounds, potentially including some naphthenic rings. These carbon blacks, formed with different fuel sources are compared using the following analytical techniques for their morphology and nanostructure

Electron Energy Loss Spectroscopy (EELS)
Fringe Analysis
Thermogravimetric Analysis
Laser Annealing
Carbon Black Aggregate Morphology and Particle Structure
Carbon Black Nanostructure
Lattice Fringe Analysis
Carbon Black Formation—Dependence upon Fuel Compositional Differences
FCC-CB
Laser Heat Treatment
Summary
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