Abstract:Laboratory-generated synthetic soot from benzene and benzene-thiophene was neodymium-doped yttrium aluminum garnet (Nd:YAG) laser and furnace annealed. Furnace annealing of sulfur doped synthetic soot resulted in the formation of micro-cracks due to the high pressures caused by explosive sulfur evolution at elevated temperature. The heteroatom sulfur affected the carbon nanostructure in a different way than oxygen. Sulfur is thermally stable in carbon up to~1000 • C and thus, played little role in the initial … Show more
“…Experimental data show that during carbonization, most of the initial oxygen in the raw materials is lost at the beginning of pyrolysis (lower temperature region), and hence the intermediate species formed after oxygen evolution dictate the resulting carbon skeleton structure and thus its ability to graphitize [25]. Unlike oxygen, nitrogen and sulfur are thermally more stable in the carbon scaffold, and hence they affect the carbon structure in a very different way than oxygen [26,27]. They play a limited role in the initial low-temperature carbonization.…”
Three types of cross-linked porous organic polymers (either oxygen-, nitrogen-, or sulfur-doped) were carbonized under a chlorine atmosphere to obtain chars in the form of microporous heteroatom-doped carbons. The studied organic polymers constitute thermosetting resins obtained via sol-gel polycondensation of resorcinol and five-membered heterocyclic aldehydes (either furan, pyrrole, or thiophene). Carbonization under highly oxidative chlorine (concentrated and diluted Cl2 atmosphere) was compared with pyrolysis under an inert helium atmosphere. All pyrolyzed samples were additionally annealed under NH3. The influence of pyrolysis and additional annealing conditions on the carbon materials’ porosity and chemical composition was elucidated.
“…Experimental data show that during carbonization, most of the initial oxygen in the raw materials is lost at the beginning of pyrolysis (lower temperature region), and hence the intermediate species formed after oxygen evolution dictate the resulting carbon skeleton structure and thus its ability to graphitize [25]. Unlike oxygen, nitrogen and sulfur are thermally more stable in the carbon scaffold, and hence they affect the carbon structure in a very different way than oxygen [26,27]. They play a limited role in the initial low-temperature carbonization.…”
Three types of cross-linked porous organic polymers (either oxygen-, nitrogen-, or sulfur-doped) were carbonized under a chlorine atmosphere to obtain chars in the form of microporous heteroatom-doped carbons. The studied organic polymers constitute thermosetting resins obtained via sol-gel polycondensation of resorcinol and five-membered heterocyclic aldehydes (either furan, pyrrole, or thiophene). Carbonization under highly oxidative chlorine (concentrated and diluted Cl2 atmosphere) was compared with pyrolysis under an inert helium atmosphere. All pyrolyzed samples were additionally annealed under NH3. The influence of pyrolysis and additional annealing conditions on the carbon materials’ porosity and chemical composition was elucidated.
“…These authors showed that carbon nanostructures produced from the nitrogen-containing precursors displayed greater curvature, and they suggested that this was because the presence of nitrogen facilitated pentagon formation. Similarly, recent work by Abrahamson and Vander Wal has shown that annealing of sulphur-doped synthetic soot can result in curvature of the carbon structure, which may be due to the formation of non-hexagonal carbon rings [46].…”
Section: The Effect Of Precursor Chemistry On Graphitizabilitymentioning
Non-graphitizing carbon, or char, has been intensively studied for decades, but there is still no agreement about its detailed atomic structure. The first models for graphitizing and non-graphitizing carbons were proposed by Rosalind Franklin in the early 1950s, and while these are correct in a broad sense, they are incomplete. Subsequent models also fail to explain fully the structure of non-graphitizing carbons. The discovery of the fullerenes and related structures stimulated the present author and others to put forward models which incorporate non-hexagonal rings into hexagonally-bonded sp2 carbon networks, creating a microporous structure made up of highly curved fragments. However, this model has not been universally accepted. This paper reviews the models that have been put forward for non-graphitizing carbon and outlines the evidence for a fullerene-like structure. This evidence comes from transmission electron microscopy, electron energy loss spectroscopy and Raman spectroscopy. Finally, the influence of precursor chemistry on the structure of graphitizing and non-graphitizing carbons is discussed. It is well established that carbonization of oxygen–containing precursors tends to produce non-graphitizing carbons. This may be explained by the fact that the removal of oxygen from a hexagonal carbon network can result in the formation of pentagonal carbon rings.
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