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Amorphous carbon nanofibers (CNFs), produced by the polymer blend technique, are activated by CO2 (ACNFs). Monoliths are synthesized from the precursor and from some ACNFs. Morphology and textural properties of these materials are studied. When compared with other activating agents (steam and alkaline hydroxides), CO2 activation renders suitable yields and, contrarily to most other precursors, turns out to be advantageous for developing and controlling their narrow microporosity (< 0.7 nm), VDR(CO2). The obtained ACNFs have a high compressibility and, consequently, a high packing density under mechanical pressure which can also be maintained upon monolith synthesis. H2 adsorption is measured at two different conditions (77 K / 0.11 MPa, and 298 K / 20 MPa) and compared with other activated carbons. Under both conditions, H2 uptake depends on the narrow microporosity of the prepared ACNFs. Interestingly, at room temperature these ACNFs perform better than other activated carbons, despite their lower porosity developments. At 298 K they reach a H2 adsorption capacity as high as 1.3 wt.%, and a remarkable value of 1 wt.% in its mechanically resistant monolith form.

In the present work we study the hydroxide activation (NaOH and KOH) of phenol-formaldehyde resin derived CNFs prepared by a polymer blend technique to prepare highly porous activated carbon nanofibres (ACNFs). Morphology and textural characteristics of these ACNFs were studied and their hydrogen storage capacities at 77 K (at 0.1 MPa and at high pressures up to 4 MPa) were assessed, and compared, with reported capacities of other porous carbon materials. Phenol-formaldehyde resin derived carbon fibres were successfully activated with these two alkaline hydroxides rendering highly microporous ACNFs with reasonable good activation process yields up to 47 wt.% compared to 7 wt.% yields from steam activation for similar surface areas of 1500 m2/g or higher. These nano-sized activated carbons present interesting H2 storage capacities at 77 K which are comparable, or even higher, to other high quality microporous carbon materials. This observation is due, in part, to their nano-sized diameters allowing to enhance their packing densities to 0.71 g/cm3 and hence their resulting hydrogen storage capacities.