, Volume 21, Issue 3, pp 1289–1303 | Cite as

Multi-technique surface characterization of bio-based films from sisal cellulose and its esters: a FE-SEM, μ-XPS and ToF-SIMS approach

  • Bruno V. M. Rodrigues
  • Elina Heikkilä
  • Elisabete Frollini
  • Pedro Fardim
Original Paper


Bio-based films were prepared from LiCl/DMAc solutions containing sisal cellulose esters (acetates, butyrates and hexanoates) with different degrees of substitution (DS 0.7–1.8) and solutions prepared with the cellulose esters and 20 wt% sisal cellulose. A novel approach for characterizing the surface morphology utilized field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), time-of-flight secondary ion mass spectrometry (ToF-SIMS) and contact angle analysis. XPS and ToF-SIMS were a powerful combination while investigating both the ester group distribution on the surface and effects of cellulose content on the film. The surface coverage by ester aliphatic chains was estimated using XPS measurements. Fibrous structures were observed in the FE-SEM images of the cellulose and bio-based films, most likely because the sisal cellulose chains aggregated during dissolution in LiCl/DMAc. Therefore, the cellulose aggregates remained after the formation of the films and removal of the solvent. The XPS results indicated that the cellulose loading on the longer chain cellulose esters films (DS 1.8) increased the surface coverage by ester aliphatic chains (8.2 % for butyrate and 45 % for hexanoate). However, for the shortest ester chains, the surface coverage decreased (acetate, 42 %). The ToF-SIMS analyses of cellulose acetate and cellulose hexanoate films (DS 1.8) revealed that the cellulose ester groups were evenly distributed across the surface of the films.


Sisal cellulose Cellulose esters films Surface analysis XPS ToF-SIMS 



The authors gratefully acknowledge FAPESP (The Sate of São Paulo Research Foundation, Brazil) for the fellowships of B. V. M. R. (proc. 2010/00005-4 and 2012/00813-9) and financial support, as well as the CNPq (National Research Council, Brazil) for the research productivity fellowship of E.F. and financial support. We also thank Top Analytica Ltd (Turku - Finland) for providing us with the XPS and ToF-SIMS instruments and M. Sc. Linus Silvander (Research Assistant at Åbo Akademi Process Chemistry Centre c/o Combustion and Materials Chemistry) for taking the FE-SEM measurements.


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Copyright information

© Springer Science+Business Media Dordrecht 2014

Authors and Affiliations

  1. 1.Macromolecular Materials and Lignocellulosic Fibers Group, Center for Research on Science and Technology of BioResources, Institute of Chemistry of São CarlosUniversity of São PauloSão CarlosBrazil
  2. 2.Laboratory of Fibre and Cellulose TechnologyÅbo Akademi UniversityTurku/ÅboFinland
  3. 3.Center of Excellence for Advanced Materials Research (CEAMR)King Abdulaziz UniversityJiddaSaudi Arabia

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