Role of annealing temperature on cation ordering in hydrothermally prepared zinc aluminate (ZnAl2O4) spinel

Journal Article · Thu Feb 15 00:00:00 EST 2018 · Materials Research Bulletin

DOI:https://doi.org/10.1016/J.MATERRESBULL.2017.10.010· OSTI ID:22805390

Dwibedi, Debasmita; Murugesan, Chinnasamy ^[1]; Leskes, Michal ^[2]; Barpanda, Prabeer ^[1]

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1. Faraday Materials Laboratory, Materials Research Center, Indian Institute of Science, C.V. Raman Avenue, Bangalore 560012 (India)
2. Department of Materials and Interfaces, Weizmann Institute of Science, Rehovot 76100 (Israel)

Highlights: • Investigation of the structural anomaly in Zinc Aluminate Spinel/ZAS (ZnAl{sub 2}O{sub 4}) by chemically inducing the defects by annealing temperature and synthetic pressure. • Hydrothermal synthesis of ZnAl{sub 2}O{sub 4} at 240 °C from nitrate precursors. • Study of the role of annealing temperature (300–900 °C) in tuning cation ordering. • Rietveld analysis of powder X-ray diffraction patterns and Raman spectroscopy to showcase disorder-order transition in ZnAl{sub 2}O{sub 4} spinels. - Abstract: Spinels (AB{sub 2}O{sub 4}) form a niche class of ceramics, which is rich in structural (dis)ordering due to the inherent mixing between the constituent tetrahedral and octahedral sites. The cations (A and B) can form antisite defects under the influence of external parameters like pressure, temperature and nuclear irradiation. The current study reports the formation and evolution of disorder-order structural transition in hydrothermally prepared zinc aluminate spinel ZnAl{sub 2}O{sub 4}. The effect of final calcination temperature (300–900 °C for 9 h) on the degree of cation ordering has been investigated with powder X-ray diffraction, Raman and {sup 27}Al solid-state NMR spectroscopy. Rietveld refinement revealed a gradual disorder to order structural transition accompanied by lower inversion parameter (i{sub s}) and smaller lattice parameter (a) with higher calcination temperature. It was further affirmed by Raman analysis and solid-state NMR spectroscopy probing the ZnO{sub 4} and AlO{sub 4} tetrahedra in spinel. Independent of the degree of cation ordering, nanometric particle size with high surface area was observed in ZnAl{sub 2}O{sub 4} spinel.

• OSTI ID: 22805390
• Journal Information: Materials Research Bulletin, Vol. 98; Other Information: Copyright (c) 2017 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; Country of input: International Atomic Energy Agency (IAEA); ISSN 0025-5408
• Country of Publication: United States
• Language: English

Related Subjects

75 CONDENSED MATTER PHYSICS
SUPERCONDUCTIVITY AND SUPERFLUIDITY
ALUMINATES
ALUMINIUM 27
ALUMINIUM OXIDES
ANNEALING
CALCINATION
CATIONS
CERAMICS
DEFECTS
HYDROTHERMAL SYNTHESIS
LATTICE PARAMETERS
NANOSTRUCTURES
NITRATES
NUCLEAR MAGNETIC RESONANCE
PARTICLE SIZE
PRESSURE DEPENDENCE
RADIATION EFFECTS
RAMAN SPECTROSCOPY
SPINELS
SURFACE AREA
TEMPERATURE DEPENDENCE
X-RAY DIFFRACTION
ZINC COMPOUNDS