Abstract
The effects of variable ionic liquid (IL) treatment time (1 s–60 min) on macroscale morphology evolution in biphasic cellulose xerogels were measured using nitrogen gas physisorption and Raman spectroscopy. Nitrogen gas adsorption/desorption measured a constant pore size (~ 12.5 nm diameter) in the xerogel phase and increasing BET surface area from 0.2 to 148.5 m2g−1 with increasing IL treatment time. Cellulose decrystallization and epoxy penetration measured using Raman spectroscopy confirmed that the xerogel phase is continuous and composed of decrystallized regenerated cellulose. The porosity of the xerogel phase (ϕV,S) decreased from 0.89 to 0.57 while the full sample porosity (ϕV,T) increased from 0.34 to 0.50 with increasing IL treatment time. Three regimes were identified to describe the propagation and growth of the regenerated xerogel cellulose phase—Regime A, Regime B, and Regime C. These results are compared with non-porous samples formed using the same IL treatment conditions to elucidate the role of solvent exchange on cellulose regeneration in these heterogeneous materials.
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Acknowledgments
This work was funded by the Air Force Office of Scientific Research [MIPR# F4FGA08354G001]. Any opinions, findings, conclusions, or recommendations expressed herein are those of the authors and do not necessarily reflect the views of the U.S. Navy or U.S. Air Force. The authors would like to thank Jeremiah Woodcock for his insightful discussions.
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Air Force Office of Scientific Research, F4FGA08354G001, Paul C. Trulove
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AA, PhD, Conceptualization; Design of experiment scheme, sample fabrication, and sample preparation (e.g., microtoming); gas sorption and optical imaging data collection and analysis; experimental calculations (i.e., cross-sectional area, porosity); Writing of the paper and cartoon creation. TC, PhD, Methodology design, data collection, and analysis of optical imaging and Raman spectroscopy data. DPD, PhD, Funding acquisition; Experimental program supervision. Prof. PCT, Funding acquisition; Experimental program supervision.
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Aiello, A., Cosby, T., Durkin, D.P. et al. Macroscale time-dependent ionic liquid treatment effects on biphasic cellulose xerogels. Cellulose 29, 8695–8704 (2022). https://doi.org/10.1007/s10570-022-04801-5
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DOI: https://doi.org/10.1007/s10570-022-04801-5