Synthesis and Characterisation of Polyol-Capped Transition Metal Oxide Nanoparticles

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Abstract:

In-situ capped nanocrystalline -Fe2O3, Co3O4, and Cu2O were prepared in 1,4-butanediol in aerobic conditions. X-ray diffraction (XRD)patterns show that the synthesised samples are nanocrystalline cubic oxides with crystallitesizes 9.5 nm, 13.4 nm, and 11 nm, respectively. Raman spectroscopy shows peaks at 350 cm−1, 500 cm−1, and 700 cm−1, indicating that the iron oxide is-Fe2O3; Mössbauer spectroscopy shows the presence of twoFe3+ sites. Transmission electron microscopy images show that the particle sizes of -Fe2O3 and Co3O4 samples are 8.9 nm and 7 nm, respectively. The absence of agglomeration indicates that the synthesised nanoparticles are capped.FT-IR spectra show the presence of an organic moiety in the sample which acts as a capping agent. Thermogravimetry showsthat the capping is stable up to 873 K in -Fe2O3, and up to 400 K in Co3O4. The samples are soluble in water to form stablehydrosols. During synthesis of -Fe2O3 a 6-line ferrihydrite is formed as an intermediate, which is stable in solution up to 473 K, and transforms to -Fe2O3 at 483 K, by rapid dissolution-reprecipitation. In the syntheses of Co3O4andCu2O, no intermediates are formed.

Keywords: CAPPING; CO3O4; CU2O; FERRIHYDRITE; GAMMA-FE2O3; NANOCRYSTALLINE; POLYOL SYNTHESIS

Document Type: Research Article

DOI: http://dx.doi.org/10.1166/jnn.2005.085

Publication date: April 1, 2005

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  • Journal for Nanoscience and Nanotechnology (JNN) is an international and multidisciplinary peer-reviewed journal with a wide-ranging coverage, consolidating research activities in all areas of nanoscience and nanotechnology into a single and unique reference source. JNN is the first cross-disciplinary journal to publish original full research articles, rapid communications of important new scientific and technological findings, timely state-of-the-art reviews with author's photo and short biography, and current research news encompassing the fundamental and applied research in all disciplines of science, engineering and medicine.
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