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Tunable mixed amorphous–crystalline cellulose substrates (MACS) for dynamic degradation studies by atomic force microscopy in liquid environments

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Abstract

Atomic force microscopy in liquid environments (L-AFM) became a state of the art technique in the field of enzymatic cellulose degradation due to its capability of in situ investigations on enzymatic relevant scales. Current investigations are however limited to few substrates like valonia cellulose, cotton linters and processed amorphous cellulose as only these show required flatness and purity. Structurally monophasic, these substrates confine conclusions regarding enzymatic degradation of mixed amorphous–crystalline substrates as commonly found in nature. To exploit the full potential of the technique, cellulose substrates with multiphase properties, flat topology and purity are therefore absolutely required. In this study we introduce a special preparation route based on highly crystalline Avicel PH101® cellulose and the ionic liquid 1-butyl-3-methylimmidazolium chloride as dissolution reagent. As comprehensively shown by atomic force microscopy, wide angle X-ray scattering, Raman spectroscopy and electron microscopy, the developed material allows precise control of its polymorphic composition by means of cellulose types I and II embedded in an amorphous matrix. Together with the tunable composition and flat topology over large areas (>10 × 10 µm2) the material is highly suited for L-AFM studies.

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Abbreviations

MACS:

Mixed amorphous−crystalline cellulose substrate

C1β :

Cellulose Iβ

C2:

Cellulose II

Avicel:

Avicel PH101®

BmimCl:

1-Butyl-3-methylimmidazolium chloride

UM:

Ultramicrotomy

L-AFM:

Atomic force microscopy in liquid environments

WAXS:

Wide angle X-ray scattering

TEM:

Transmission electron microscopy

SEM:

Scanning electron microscopy

RS:

Raman spectroscopy

RMS:

Root mean square roughness

FWHM:

Full width at half maximum

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Acknowledgments

We thank Stefan Mitsche for helping us with WAXS analysis; Stephanie Rosker for helping us with the experiments; Angelina Orthacker, Robert Winkler and Ferdinand Hofer for discussions. Gratitude goes to the Cambridge Crystallographic Data Centre (CCDC) for the ability to use Mercury 3.3 for simulation purposes. Financial support was provided from the Austrian Science Fund FWF (Grant P 24156-B21 to B.N.).

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Authors and Affiliations

  1. Institute for Electron Microscopy and Nanoanalysis, Graz University of Technology, Steyrergasse 17, 8010, Graz, Austria

    Thomas Ganner, Timothy Aschl & Harald Plank

  2. Institute of Biotechnology and Biochemical Engineering, Graz University of Technology, Petersgasse 12, 8010, Graz, Austria

    Manuel Eibinger, Patricia Bubner & Bernd Nidetzky

  3. Graz Centre for Electron Microscopy, Steyrergasse 17, 8010, Graz, Austria

    Arno Meingast, Boril Chernev, Claudia Mayrhofer & Harald Plank

  4. Austrian Centre of Industrial Biotechnology, Petersgasse 14, 8010, Graz, Austria

    Bernd Nidetzky

Authors
  1. Thomas Ganner
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  2. Timothy Aschl
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  3. Manuel Eibinger
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  4. Patricia Bubner
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  9. Harald Plank
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Corresponding authors

Correspondence to Bernd Nidetzky or Harald Plank.

Additional information

Thomas Ganner and Timothy Aschl have contributed equally to this work.

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Ganner, T., Aschl, T., Eibinger, M. et al. Tunable mixed amorphous–crystalline cellulose substrates (MACS) for dynamic degradation studies by atomic force microscopy in liquid environments. Cellulose 21, 3927–3939 (2014). https://doi.org/10.1007/s10570-014-0419-8

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  • DOI: https://doi.org/10.1007/s10570-014-0419-8

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