Thermo-Raman spectroscopy in situ monitoring study of solid-state synthesis of NiO-Al{sub 2}O{sub 3} nanoparticles and its characterization

Journal Article · Tue Dec 15 00:00:00 EST 2009 · Journal of Solid State Chemistry

DOI:https://doi.org/10.1016/j.jssc.2009.09.019· OSTI ID:21372439

Ghule, Kalyani; Tzing, S -H; Punde, Tushar H; Hua, Chang ^[1]

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1. Department of Chemistry, National Tsing Hua University, Hsinchu, Taiwan-300 (China)

Hyphenation of thermogravimetric analyzer (TGA) and thermo-Raman spectrophotometer for in situ monitoring of solid-state reaction in oxygen atmosphere forming NiO-Al{sub 2}O{sub 3} catalyst nanoparticles is investigated. In situ thermo-Raman spectra in the range from 200 to 1400 cm{sup -1} were recorded at every degree interval from 25 to 800 deg. C. Thermo-Raman spectroscopic studies reveal that, although the onset of formation is around 600 deg. C, the bulk NiAl{sub 2}O{sub 4} forms at temperatures above 800 deg. C. The X-ray diffraction (XRD) spectra and the scanning electron microscopy (SEM) images of the reaction mixtures were recorded at regular temperature intervals of 100 deg. C, in the temperature range from 400 to 1000 deg. C, which could provide information on structural and morphological evolution of NiO-Al{sub 2}O{sub 3}. Slow controlled heating of the sample enabled better control over morphology and particle size distribution ({approx}20-30 nm diameter). The observed results were supported by complementary characterizations using TGA, XRD, SEM, transmission electron microscopy, and energy dispersive X-ray analysis. - Graphical abstract: Hyphenation of thermogravimetric analyzer and thermo-Raman spectrophotometer for in situ monitoring of solid-state reaction at controlled heating rate and in oxygen atmosphere forming NiO-Al{sub 2}O{sub 3} catalyst nanoparticles is investigated.

• OSTI ID: 21372439
• Journal Information: Journal of Solid State Chemistry, Vol. 182, Issue 12; Other Information: DOI: 10.1016/j.jssc.2009.09.019; PII: S0022-4596(09)00454-X; Copyright (c) 2009 Elsevier Science B.V., Amsterdam, The Netherlands, All rights reserved.; ISSN 0022-4596
• Country of Publication: United States
• Language: English

Related Subjects

77 NANOSCIENCE AND NANOTECHNOLOGY
ALUMINIUM OXIDES
NANOSTRUCTURES
NICKEL OXIDES
RAMAN SPECTROSCOPY
SCANNING ELECTRON MICROSCOPY
TEMPERATURE RANGE 0273-0400 K
TEMPERATURE RANGE 0400-1000 K
TEMPERATURE RANGE 1000-4000 K
THERMAL GRAVIMETRIC ANALYSIS
X-RAY DIFFRACTION
ALUMINIUM COMPOUNDS
CHALCOGENIDES
CHEMICAL ANALYSIS
COHERENT SCATTERING
DIFFRACTION
ELECTRON MICROSCOPY
GRAVIMETRIC ANALYSIS
LASER SPECTROSCOPY
MICROSCOPY
NICKEL COMPOUNDS
OXIDES
OXYGEN COMPOUNDS
QUANTITATIVE CHEMICAL ANALYSIS
SCATTERING
SPECTROSCOPY
TEMPERATURE RANGE
THERMAL ANALYSIS
TRANSITION ELEMENT COMPOUNDS