A method was developed to deagglomerate commercially available multi-walled carbon nanotube (MWCNT) bundles while maintaining the carbon nanotube aspect ratio. The process utilizes the rapid expansion of a supercritical carbon dioxide/MWCNT mixture to separate large primary carbon nanotube agglomerates. High levels of deagglomeration of Baytubes Ò C 150 P and Nanocyl TM NC-7000 MWCNT bundles were observed on the macroscale and nanoscale, resulting in 30-fold and 50-fold decreases in bulk density, respectively, with median agglomerate sizes \8 lm in diameter. These results were obtained while retaining the aspect ratio of the as-received nanomaterial, irrespective of the MWCNT agglomerate morphology. It was found that a temperature and pressure of 40°C and 7.86 MP resulted in maximum deagglomeration without damage to the MWCNTs. Thermodynamic principles were applied to describe the effect of processing variables on the efficiency of the deagglomeration. These results suggest that combining this process with a composite processing step, such as melt compounding, will result in nanocomposites with enhanced electrical properties.