Low temperature superparamagnetic nanocomposites obtained by Fe(acac)3-SiO2-PVA hybrid xerogel thermolysis

Author:

Ianasi Catalin1,Costisor Otilia1,Putz Ana-Maria1,Lazau Radu2,Negrea Adina2,Niznansky Daniel3,Sacarescu Liviu4,Savii Cecilia1

Affiliation:

1. Institute of Chemistry Timisoara of Romanian Academy, Timisoara, Romania

2. Polytechnic University Timisoara, Faculty of Chemistry and Environmental Engineering, Timisoara, Romania

3. Charles University in Prague, Faculty of Science, Department of Inorganic Chemistry, Prague, Czech Republic

4. Institute of Macromolecular Chemistry “Petru Poni”, Iasi, Romania

Abstract

Fe(acac)3/silica/PVA hybrid xerogel nanocomposite was obtained by one pot acid catalysed sol-gel synthesis using the homogeneous mixture of iron(III) acetylacetonate (Fe(acac)3), tetraethylorthosilicate (TEOS), and polyvinyl alcohol (PVA). Nominal composition ratio of iron oxide/silica was 15/85 (weight percent). Nitric acid was used as catalyst. Another sample of Fe(acac)3/silica xerogel without PVA addition was prepared in the similar processing conditions. Based on thermal analysis studies, the thermal behaviour of both xerogel samples was unveiled and it allowed choosing the optimal calcination temperatures in order to obtain iron oxide silica magnetic nanocomposite samples. The two xerogel (with and without PVA) samples were thermally treated, in air, at 220, 260 and 300?C and characterized by different techniques. XRD investigations revealed phase composition evolution with calcination temperature, from cubic spinel phase (maghemite) to hexagonal stable hematite containing nanocomposite of 10-20 nm average crystallite size. These findings were confirmed by M?ssbauer spectroscopy. Up to 300?C, the surface area and total pores volume increased with temperature for all samples. By calcination at the same temperature, the hybrid xerogel containing PVA resulted in significantly higher magnetization and free volume values in comparison with the sample without PVA.

Publisher

National Library of Serbia

Subject

Ceramics and Composites

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