Ultrasound-enhanced milling in the synthesis of phase-pure, highly crystalline ZnAl-layered double hydroxide of low Zn(II) content--颗粒学报PARTICUOLOGY

Szabados, M., Bús, C., Ádok-Sipiczki, M., Kónya, Z., Kukovecz, Á., Sipos, P., & Pálinkó, I. (2016). Ultrasound-enhanced milling in the synthesis of phase-pure, highly crystalline ZnAl-layered double hydroxide of low Zn(II) content. Particuology, 27, 29-33. https://doi.org/10.1016/j.partic.2016.01.006

Ultrasound-enhanced milling in the synthesis of phase-pure, highly crystalline ZnAl-layered double hydroxide of low Zn(II) content

M. Szabados ^{a b}, Cs. Bús ^{a b}, M. Ádok-Sipiczki ^{a b}, Z. Kónya ^{c d}, Á. Kukovecz ^c^e, P. Sipos ^{b f}, I. Pálinkó ^{a b *}

a Department of Organic Chemistry, University of Szeged, Dómtér 8, Szeged H-6720, Hungary
b Material and Solution Structure Research Group, Institute of Chemistry, University of Szeged, Aradi Vértanúk tere 1, Szeged H-6720, Hungary
c Department of Applied and Environmental Chemistry, University of Szeged, Rerrich B. tér 1, Szeged H-6720, Hungary
d MTA-SZTE Reaction Kinetics and Surface Chemistry Research Group, Rerrich B tér 1, Szeged H-6720, Hungary
e MTA-SZTE “Lendület” Porous Nanocomposites Research Group, Rerrich B. tér 1, Szeged H-6720, Hungary
f Department of Inorganic and Analytical Chemistry, University of Szeged, Dómtér 7, Szeged H-6720, Hungary

10.1016/j.partic.2016.01.006

Volume 27, August 2016, Pages 29-33

Received 19 December 2015, Revised 17 January 2016, Accepted 26 January 2016, Available online 2 May 2016, Version of Record 14 June 2016.

E-mail: palinko@chem.u-szeged.hu

Highlights

• ZnAl-layered double hydroxide (LDH) was synthesised by ultrasonically enhanced milling.

• Optimum synthetic conditions were identified.

• Phase-pure ZnAl-LDH with high crystallinity was obtained by rinsing the product with aqueous NH₃.

Abstract

Dry milling followed by ultrasonic irradiation in the presence of small amounts of aqueous NaOH, was used to synthesise ZnAl-layered double hydroxide (LDH). The synthetic conditions were optimised and the Zn(OH)₂, ZnO, and Al(OH)₃ contaminants were removed by rinsing with aqueous NH₃ solution from the sample prepared in the optimum conditions. Thus, phase-pure ZnAl-layered double hydroxide was obtained with high crystallinity. All materials produced during the syntheses were characterised by X-ray diffractometry, and a rose-like morphology was observed by scanning electron microscopy in the phase-pure sample. By changing the initial Zn/Al ratio, it was revealed that an LDH with low zinc content was always formed, probably through substitution of some of the Zn²⁺ ions by Al³⁺ ions in the gibbsite lattice.

Graphical abstract

Keywords

ZnAl-layered double hydroxide; Dry milling; Ultrasonic irradiation

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