We
report a sustainable and easy approach for the preparation of
cellulose-based aerogels from the DBU–CO2 switchable
solvent system via a solubilization and coagulation approach followed
by freeze-drying. The easy, fast, and mild solubilization step (15
min at 30 °C) allows for a rapid preparation procedure. The effect
of various processing parameters, such as cellulose concentration,
coagulating solvent, and the superbase, on important aerogel characteristics
including density, porosity, pore size, and morphology, were investigated.
Density values obtained ranged between 0.05 and 0.12 g/cm3, with porosity values between 92% and 97%. The morphology of the
obtained cellulose aerogels was studied using scanning electron microscopy
(SEM) showing a random and open large macroporous cellulose network
with pore sizes ranging between 1.1 and 4.5 μm, depending on
the processing conditions. In addition, specific surface areas determined
by N2 adsorption applying the BET equation ranged between
19 and 26 m2/g. The effect of the coagulating solvent and
superbase on the crystallinity was investigated using X-ray diffraction
(XRD) showing an amorphous crystal structure with a broad 2θ
diffraction peak at 20.6°. In addition, no chemical modification
was observed in the prepared aerogels from infrared spectroscopy.
Finally, the recovery and reuse of the solvent system was demonstrated,
thus making the process more sustainable.
In Part A of this study, infiltrations experiments of porous SiC samples by hexadecane with poresize distributions comprising small and large pores were realized. Two successive stages were identified during the filling of these samples corresponding to the infiltration of the two types of pores. The experimental data were successfully treated with a new analytical function. In Part B, it was found that this function can also be applied to the analysis of the mass gain during molten silicon infiltration at 1500°C. Prior to silicon infiltration, it was found that the operating temperature induces a shift of the pore size distributions towards larger values. A dissolutionrecrystallisation mechanism can also occur during the infiltration of silicon. During the first stage, liquid silicon fills rapidly larger pores than hexadecane. The kinetics are significantly larger with liquid silicon. Consequently, the durations for the complete filling are very short with molten silicon.
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