Surface Characterization of Mechanochemically Modified Exfoliated Halloysite Nanoscrolls

Balázs Zsirka, Attila Táborosi, Péter Szabó, Róbert K. Szilágyi, E. Horváth, Tatjána Juzsakova, Dávid Fertig, J. Kristóf

Research output: Contribution to journalArticle

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Abstract

Surface modifications fundamentally influence the morphology of kaolinite nanostructures as a function of crystallinity and the presence of contaminants. Besides morphology, the catalytic properties of 1:1-type exfoliated aluminosilicates are also influenced by the presence of defect sites that can be generated in a controlled manner by mechanochemical activation. In this work, we investigated exfoliated halloysite nanoparticles with a quasi-homogeneous, scroll-type secondary structure toward developing structural/functional relationships for composition, atomic structure, and morphology. The surface properties of thin-walled nanoscrolls were studied as a function of mechanochemical activation expressed by the duration of dry-grinding. The surface characterizations were carried out using N2, NH3, and CO2 adsorption measurements. The effects of grinding on the nanohalloysite structure were followed using thermoanalytical thermogravimetric/derivative thermogravimetric (TG/DTG) and infrared spectroscopic [Fourier transform infrared/attenuated total reflection (FTIR/ATR)] techniques. Grinding results in partial dehydroxylation with similar changes as those observed for heat treatment above 300 °C. Mechanochemical activation shows a decrease in the dehydroxylation mass loss and the DTG peak temperature, a decrease in the specific surface area and the number of mesopores, an increase in the surface acidity, blue shift of surface hydroxide bands, and a decrease in the intensity of FTIR/ATR bands as a function of the grinding time. The experimental observations were used to guide atomic-scale structural and energetic simulations using realistic molecular cluster models for a nanohalloysite particle. A full potential energy surface description was developed for the mechanochemical activation and/or heating toward nanometahalloysite formation that aids the interpretation of experimental results. The calculated differences upon dehydroxylation show a remarkable agreement with the mass loss values from DTG measurements.

Original languageEnglish
Pages (from-to)3534-3547
Number of pages14
JournalLangmuir
Volume33
Issue number14
DOIs
Publication statusPublished - Apr 11 2017

Fingerprint

Chemical activation
grinding
Infrared radiation
activation
Fourier transforms
Kaolin
Potential energy surfaces
Kaolinite
Aluminosilicates
Acidity
Specific surface area
Surface properties
Surface treatment
Nanostructures
molecular clusters
kaolinite
Heat treatment
Impurities
Nanoparticles
Derivatives

ASJC Scopus subject areas

  • Materials Science(all)
  • Condensed Matter Physics
  • Surfaces and Interfaces
  • Spectroscopy
  • Electrochemistry

Cite this

Surface Characterization of Mechanochemically Modified Exfoliated Halloysite Nanoscrolls. / Zsirka, Balázs; Táborosi, Attila; Szabó, Péter; Szilágyi, Róbert K.; Horváth, E.; Juzsakova, Tatjána; Fertig, Dávid; Kristóf, J.

In: Langmuir, Vol. 33, No. 14, 11.04.2017, p. 3534-3547.

Research output: Contribution to journalArticle

Zsirka, B, Táborosi, A, Szabó, P, Szilágyi, RK, Horváth, E, Juzsakova, T, Fertig, D & Kristóf, J 2017, 'Surface Characterization of Mechanochemically Modified Exfoliated Halloysite Nanoscrolls', Langmuir, vol. 33, no. 14, pp. 3534-3547. https://doi.org/10.1021/acs.langmuir.6b04606
Zsirka, Balázs ; Táborosi, Attila ; Szabó, Péter ; Szilágyi, Róbert K. ; Horváth, E. ; Juzsakova, Tatjána ; Fertig, Dávid ; Kristóf, J. / Surface Characterization of Mechanochemically Modified Exfoliated Halloysite Nanoscrolls. In: Langmuir. 2017 ; Vol. 33, No. 14. pp. 3534-3547.
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