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Advanced microscopy and spectroscopy reveal the adsorption and clustering of Cu(II) onto TEMPO-oxidized cellulose nanofibers
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Luleå University of Technology, Sweden.
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK). Luleå University of Technology, Sweden.
Number of Authors: 3
2017 (English)In: Nanoscale, ISSN 2040-3364, E-ISSN 2040-3372, Vol. 9, no 22, p. 7419-7428Article in journal (Refereed) Published
Abstract [en]

TEMPO (2,2,6,6-tetramethylpiperidine-1-oxylradical)-mediated oxidation nanofibers (TOCNF), as a biocompatible and bioactive material, have opened up a new application of nanocellulose for the removal of water contaminants. This development demands extremely sensitive and accurate methods to understand the surface interactions between water pollutants and TOCNF. In this report, we investigated the adsorption of metal ions on TOCNF surfaces using experimental techniques atthe nano and molecular scales with Cu(II) as the target pollutant in both aqueous and dry forms. Imaging with in situ atomic force microscopy (AFM), together with a study of the physiochemical properties of TOCNF caused by adsorption with Cu(II) in liquid, were conducted using the PeakForce Quantitative NanoMechanics (PF-QNM) mode at the nano scale. The average adhesion force between the tip and the target single TOCNF almost tripled after adsorption with Cu(II) from 50 pN to 140 pN. The stiffness of the TOCNF was also enhanced because the Cu(II) bound to the carboxylate groups and hardened the fiber. AFM topography, scanning electron microscopy-energy dispersive X-ray spectroscopy (SEM-EDS) mapping and X-ray photoelectron spectroscopy (XPS) indicated that the TOCNF were covered by copper nanolayers and/or nanoparticles after adsorption. The changes in the molecular structure caused by the adsorption were demonstrated by Raman and attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). This methodology will be of great assistance to gain qualitative and quantitative information on the adsorption process and interaction between charged entities in aqueous medium.

Place, publisher, year, edition, pages
2017. Vol. 9, no 22, p. 7419-7428
National Category
Chemical Sciences
Research subject
Materials Chemistry
Identifiers
URN: urn:nbn:se:su:diva-144778DOI: 10.1039/c7nr01566fISI: 000402881600009OAI: oai:DiVA.org:su-144778DiVA, id: diva2:1127550
Available from: 2017-07-17 Created: 2017-07-17 Last updated: 2018-04-23Bibliographically approved
In thesis
1. Nanocellulose and Its Biohybrids for Water Purification: Atomic Force Microscopy as a Tool to Probe Surface Properties and Interactions
Open this publication in new window or tab >>Nanocellulose and Its Biohybrids for Water Purification: Atomic Force Microscopy as a Tool to Probe Surface Properties and Interactions
2018 (English)Doctoral thesis, comprehensive summary (Other academic)
Abstract [en]

Nanocellulose has been explored extensively in recent years as an adsorbent due to its promising performance in the removal of charged contaminants from water. In this thesis, various atomic force microscopy (AFM) techniques are used to understand the surface characteristics and specific interactions of nanocellulose with water contaminants (heavy metal ions and dyes) and nanoscale entities (Graphene Oxide (GO) and Graphene Oxide nanocolloids (nanoGO)), and explain the mechanisms related to adsorption, metal ion clustering, self-assembly and mechanical reinforcement.

AFM probes functionalised with microscale and nanoscale celluloses were used as colloidal probes to study specific surface interactions with heavy metal ions and dyes in the aqueous medium. This approach enabled quantitative measurements of the adhesion force between nanocellulose and the water pollutants under in situ conditions by direct or in-direct methods. Adhesion forces, including the piconewton range, were measured, and the forces depended on the surface groups present on the nanocellulose.

AFM imaging in dry and/or wet conditions was successfully used to investigate the adsorption, self-assembly, morphology and mechanical properties of nanocellulose and its bio-hybrids. The self-assembly, the metal nanolayer and the nanoclusters on the surface of nanocellulose and its biohybrids after adsorption were confirmed and explained by advanced microscopy, spectroscopy and computational modelling.

The adhesion and stiffness measurement of single nanocellulose fibers using in situ PeakForce Quantitative Nanomechanical (PF-QNM) characterization confirmed the adsorption of metal ions on the surface in the liquid medium. PF-QNM mapping of the freestanding biohybrid membranes also revealed the enhanced modulus of the biohybrid membrane compared with the TEMPO(2,2,6,6-tetramethylpiperidine-1-oxylradical)-mediated oxidation nanofibers (TOCNF) membrane, which explained the hydrolytic stability and recyclability of these membranes.

The established methodology, which combines advanced microscopy with spectroscopy and modelling techniques, can be extended to other biobased macromolecular systems to investigate the adsorption behaviour and/or surface interactions in bio nanotechnology.

Place, publisher, year, edition, pages
Stockholm: Department of Materials and Environmental Chemistry (MMK), Stockholm University, 2018. p. 23
Keyword
Atomic force microscopy, nanocellulose, water purification, surface interaction, biohybrids, self-assembly, metal ion clustering
National Category
Materials Chemistry
Research subject
Materials Chemistry
Identifiers
urn:nbn:se:su:diva-155373 (URN)978-91-7797-260-0 (ISBN)978-91-7797-261-7 (ISBN)
Public defence
2018-06-08, Magnéli Hall, Arrhenius Laboratory, Svante Arrhenius väg 16 B, Stockholm, 09:30 (English)
Opponent
Supervisors
Note

At the time of the doctoral defense, the following papers were unpublished and had a status as follows: Paper 4: Manuscript. Paper 5: Manuscript.

Available from: 2018-05-16 Created: 2018-04-19 Last updated: 2018-05-09Bibliographically approved

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