The morphology and rheology of carbon nanofiber (CNF) suspensions were studied. The CNFs, produced by decomposing organic vapors at elevated temperature in the presence of metal catalysts, have characteristic diameter and length of 100 nm and 20–100 μm, respectively. The CNFs, as delivered, have a strong tendency to clump into mm-sized agglomerates. The efficacy of CNF/glycerol-water suspensions was studied vs. two processing parameters: mechanical sonication and chemical treatment. Experimental measurements revealed that sonication alone reduces the size of CNF clumps from millimeter to micrometer scale, but cannot achieve uniform dispersion. The chemically untreated sonicated suspensions contain clumps of nanofibers with a characteristic size of 20×50 μm, together with smaller aggregations of partially dispersed nanofibers. In response to this unsatisfactory dispersion, the effect of acid treatment before dispersion was investigated. This acid treatment, which makes the surface of the CNFs more hydrophilic, greatly improves dispersion in the aqueous solution: treatment followed by sonication results in a uniform dispersion of individual nanofibers. At the same time, however, we observed that surface treatment and subsequent sonication greatly shorten the nanofibers.