J. Drbohlav et Wtk. Stevenson, THE OXIDATIVE STABILIZATION AND CARBONIZATION OF A SYNTHETIC MESOPHASE PITCH .1. THE OXIDATIVE STABILIZATION PROCESS, Carbon, 33(5), 1995, pp. 693-711
The transformation of mesophase pitch to an ordered carbon by high-tem
perature heat treatment in an inert atmosphere must be preceded by a s
uitable period of thermosetting or oxidative stabilization. The chemic
al process of oxidative stabilization is not well characterized, altho
ugh research has clearly indicated that the oxidation history of the m
esophase has a profound impact on the mechanical qualities of the resu
ltant carbon product. In this study, we oxidized samples of a commerci
ally available, synthetic mesophase pitch to determine the effect of d
ifferent time/temperature profiles of oxidation on the quantity and ty
pe of introduced functionality. Fourier transform infrared spectroscop
y (FT-IR) was used to characterize and quantify oxygen functionality p
resent in this oxidized pitch. The oxidation process was characterized
by periods of weight gain and weight loss. It was concluded that weig
ht gain during oxidation involves the loss of aliphatic content in the
pitch, with a concurrent increase in oxygen content as predominately
ester and anhydride functionality. Weight loss is characterized by a l
oss of aromatic carbon content from the pitch and a further increase i
n the relative oxygen content in the pitch. It was discovered that cha
nging the time/temperature profile of oxidation affects the pitch prim
arily via the degree of weight gain and weight loss experienced, rathe
r than through the introduction of specific functionality-with weight
gain dominating at lower oxidation temperatures and shorter time perio
ds, and weight loss dominating at higher temperatures and longer perio
ds of oxidation. We conclude by suggesting mechanisms of derivatizatio
n to explain the oxidative stabilization of this synthetic, naphthalen
e-derived mesophase pitch in an oxygen-rich atmosphere.