Thin-walled nanoscrolls by multi-step intercalation from tubular halloysite-10 Å and its rearrangement upon peroxide treatment

Balázs Zsirka, E. Horváth, Péter Szabó, Tatjána Juzsakova, Róbert K. Szilágyi, Dávid Fertig, Éva Makó, Tamás Varga, Z. Kónya, Ákos Kukovecz, János Kristóf

Research output: Contribution to journalArticle

5 Citations (Scopus)

Abstract

Surface modification of the halloysite-10 Å mineral with tubular morphology can be achieved by slightly modified procedures developed for the delamination of kaolinite minerals. The resulting delaminated halloysite nanoparticles have unexpected surface/morphological properties that display, new potentials in catalyst development. In this work, a four-step intercalation/delamination procedure is described for the preparation of thin-walled nanoscrolls from the multi-layered hydrated halloysite mineral that consists of (1) intercalation of halloysite with potassium acetate, (2) replacement intercalation with ethylene glycol, (3) replacement intercalation with hexylamine, and (4) delamination with toluene. The intercalation steps were followed by X-ray diffraction, transmission electron microscopy, N2 adsorption-desorption, thermogravimetry, and infrared spectroscopy. Delamination eliminated the crystalline order and the crystallite size along the ‘c’-axis, increased the specific surface area, greatly decreased the thickness of the mineral tubes to a monolayer, and shifted the pore diameter toward the micropore region. Unexpectedly, the removal of residual organics from intercalation steps adsorbed at the nanoscroll surface with a peroxide treatment resulted in partial recovery of crystallinity and increase of crystallite size along the ‘c’-crystal direction. The d(001) value showed a diffuse pattern at 7.4–7.7 Å due to the rearrangement of the thin-walled nanoscrolls toward the initial tubular morphology of the dehydrated halloysite-7 Å mineral.

Original languageEnglish
Pages (from-to)245-254
Number of pages10
JournalApplied Surface Science
Volume399
DOIs
Publication statusPublished - Mar 31 2017

Fingerprint

Peroxides
Intercalation
Minerals
Delamination
Crystallite size
Potassium Acetate
Kaolin
Ethylene Glycol
Kaolinite
Toluene
Ethylene glycol
Specific surface area
Surface properties
Potassium
Surface treatment
Thermogravimetric analysis
clay
Infrared spectroscopy
Monolayers
Desorption

Keywords

  • Halloysite nanoscrolls
  • Intercalation
  • Oxidative surface cleaning
  • Rearrangement of nanostructures
  • Surface characterisation

ASJC Scopus subject areas

  • Surfaces, Coatings and Films

Cite this

Thin-walled nanoscrolls by multi-step intercalation from tubular halloysite-10 Å and its rearrangement upon peroxide treatment. / Zsirka, Balázs; Horváth, E.; Szabó, Péter; Juzsakova, Tatjána; Szilágyi, Róbert K.; Fertig, Dávid; Makó, Éva; Varga, Tamás; Kónya, Z.; Kukovecz, Ákos; Kristóf, János.

In: Applied Surface Science, Vol. 399, 31.03.2017, p. 245-254.

Research output: Contribution to journalArticle

Zsirka, Balázs ; Horváth, E. ; Szabó, Péter ; Juzsakova, Tatjána ; Szilágyi, Róbert K. ; Fertig, Dávid ; Makó, Éva ; Varga, Tamás ; Kónya, Z. ; Kukovecz, Ákos ; Kristóf, János. / Thin-walled nanoscrolls by multi-step intercalation from tubular halloysite-10 Å and its rearrangement upon peroxide treatment. In: Applied Surface Science. 2017 ; Vol. 399. pp. 245-254.
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abstract = "Surface modification of the halloysite-10 {\AA} mineral with tubular morphology can be achieved by slightly modified procedures developed for the delamination of kaolinite minerals. The resulting delaminated halloysite nanoparticles have unexpected surface/morphological properties that display, new potentials in catalyst development. In this work, a four-step intercalation/delamination procedure is described for the preparation of thin-walled nanoscrolls from the multi-layered hydrated halloysite mineral that consists of (1) intercalation of halloysite with potassium acetate, (2) replacement intercalation with ethylene glycol, (3) replacement intercalation with hexylamine, and (4) delamination with toluene. The intercalation steps were followed by X-ray diffraction, transmission electron microscopy, N2 adsorption-desorption, thermogravimetry, and infrared spectroscopy. Delamination eliminated the crystalline order and the crystallite size along the ‘c’-axis, increased the specific surface area, greatly decreased the thickness of the mineral tubes to a monolayer, and shifted the pore diameter toward the micropore region. Unexpectedly, the removal of residual organics from intercalation steps adsorbed at the nanoscroll surface with a peroxide treatment resulted in partial recovery of crystallinity and increase of crystallite size along the ‘c’-crystal direction. The d(001) value showed a diffuse pattern at 7.4–7.7 {\AA} due to the rearrangement of the thin-walled nanoscrolls toward the initial tubular morphology of the dehydrated halloysite-7 {\AA} mineral.",
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AU - Juzsakova, Tatjána

AU - Szilágyi, Róbert K.

AU - Fertig, Dávid

AU - Makó, Éva

AU - Varga, Tamás

AU - Kónya, Z.

AU - Kukovecz, Ákos

AU - Kristóf, János

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N2 - Surface modification of the halloysite-10 Å mineral with tubular morphology can be achieved by slightly modified procedures developed for the delamination of kaolinite minerals. The resulting delaminated halloysite nanoparticles have unexpected surface/morphological properties that display, new potentials in catalyst development. In this work, a four-step intercalation/delamination procedure is described for the preparation of thin-walled nanoscrolls from the multi-layered hydrated halloysite mineral that consists of (1) intercalation of halloysite with potassium acetate, (2) replacement intercalation with ethylene glycol, (3) replacement intercalation with hexylamine, and (4) delamination with toluene. The intercalation steps were followed by X-ray diffraction, transmission electron microscopy, N2 adsorption-desorption, thermogravimetry, and infrared spectroscopy. Delamination eliminated the crystalline order and the crystallite size along the ‘c’-axis, increased the specific surface area, greatly decreased the thickness of the mineral tubes to a monolayer, and shifted the pore diameter toward the micropore region. Unexpectedly, the removal of residual organics from intercalation steps adsorbed at the nanoscroll surface with a peroxide treatment resulted in partial recovery of crystallinity and increase of crystallite size along the ‘c’-crystal direction. The d(001) value showed a diffuse pattern at 7.4–7.7 Å due to the rearrangement of the thin-walled nanoscrolls toward the initial tubular morphology of the dehydrated halloysite-7 Å mineral.

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KW - Rearrangement of nanostructures

KW - Surface characterisation

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