Cellulose nanocrystals - structural insights via 2D q-mapping

Heike Ehmann

Anton Paar GmbH, Graz, Austria

Cellulose, as the most abundant biopolymer in the world, is the structural component of the primary cell wall of green plants, as well as many algae.1-3 There are various methods known which describe the extraction the crystalline regions like the here presented acidolysis which results in the formation of cellulose nanocrystals (CNC).4 CNCs are very popular in modern science due to their outstanding properties like reactivity, high surface to volume ratio, liquid crystalline behavior, colloidal stability as well as their unique mechanical properties. Cellulose occurs not only in nature but also in laboratory in many modifications and structural forms.3-4 The use of nanoscale cellulose fibers and their application in the field of composite materials has become very popular due to their high strength, stiffness, low weight, biodegradability as well as renewability.4-7

To extract these extraordinary properties, one has to break down the hierarchical structure of the plant into individualized nanofibers of high crystallinity and reduced amorphous regions. The extraction of the crystalline domains described in this work is the controlled acidolysis in sulfuric acid. The focus of this talk lies on small and wide angle X-ray scattering (SWAXS) techniques using the TrueSWAXS feature by creating a full 2D q-map of the resulting CNC species. The SAXS regime allows to assess the size and shape via the intra-particle interferences via the form factor and the also the inter-particle interferences via the so-called structure factor (interaction). Additionally the crystallinity was determined by using the 2D WAXS profile. For this purpose the device function was determined using NIST660c (LaB6) to take the peak broadening and intensity calibration into account.

[1] H.M.A. Ehmann, Ph.D. Thesis (2012) doi: 10.13140/rg.2.1.3192.6646.

[2] R. Brown et al, Proc. Nat. Acad. Sci. U.S.A 73 (1976) 4656.

[3] D. Klemm et al, Weinheim (1998) doi:10.1002/3527601929.

[4] N. Durán et al, Recent Pat Nanotechnol 6 (2012) 16.

[5] Y. Habibi et al, Chem. Rev. 110 (2010) 3479.

[6] E. Kontturi et al, Langmuir 23 (2007) 9674.

[7] H.M.A. Ehmann et al, Langmuir 29 (2013) 3740.