Understanding heat driven gelation of anionic cellulose nanofibrils: Combining Saturation Transfer Difference (STD) NMR, Small Angle X-ray Scattering (SAXS) and rheology

Vincenzo Calabrese, Juan C. Muñoz-García, Julien Schmitt, Marcelo A. da Silva, Janet L. Scott, Jesús Angulo, Yaroslav Z. Khimyak, Karen J. Edler

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A novel mechanism of heat-triggered gelation for oxidised cellulose nanofibrils (OCNF) is reported. We demonstrate that a synergistic approach combining rheology, small-angle X-ray scattering (SAXS) and saturation transfer difference NMR (STD NMR) experiments enables a detailed characterisation of gelation at different length scales. OCNF dispersions experience an increase in solid-like behaviour upon heating as evidenced by rheological studies, associated with enhanced interfibrillar interactions measured using SAXS. Interactions result in an increased fibrillar overlap and increased population of confined water molecules monitored by STD NMR. In comparison, cationic cellulose nanofibrils (produced by reaction of cellulose with trimethylglycidylammonium chloride) were found to be heat-unresponsive.

Original languageEnglish
Pages (from-to)205-213
Number of pages9
JournalJournal of Colloid and Interface Science
Early online date25 Sep 2018
Publication statusPublished - 1 Feb 2019


  • Water confinement
  • hydrogel
  • TEMPO oxidised cellulose
  • heat induced gelation
  • saturation transfer difference NMR
  • SAXS
  • rheology

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