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Journal of Materials Science

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17-02-2017 | Original Paper

Co(II) ethylene glycol carboxylates for Co₃O₄ nanoparticle and nanocomposite formation

Authors: K. Assim, S. Schulze, M. Pügner, M. Uhlemann, T. Gemming, L. Giebeler, M. Hietschold, T. Lampke, H. Lang

Published in: Journal of Materials Science | Issue 11/2017

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Abstract

Ethylene glycol-functionalized Co(II) carboxylates [Co(CO₂CH₂(OC₂H₄)_nOMe)₂] (2a, n = 1; 2b, n = 2), [Co(CO₂CHPh(OC₂H₄)₂OMe)₂] (2c) and [Co(CO₂CMe₂(O–C₂H₄)₂OMe)₂] (2d) have been synthesized by the reaction of [Co(OAc)₂·4H₂O] with the corresponding acids MeO(C₂H₄O)_nCRR′CO₂H (n = 1, 2; R=H, R′=Me; R=H, R′=Ph). Based on the IR spectroscopic studies, the binding motif of the carboxylato ligands to cobalt is discussed. Thermogravimetry and mass spectrometry studies were carried out in order to investigate the thermal decomposition mechanism of 2a–2d in the solid state. Based on the result obtained, complex 2b was chosen as single-source precursor for the generation and stabilization of Co₃O₄ nanoparticles (NPs) by solid-state thermal decomposition in air. Depending on the decomposition time, NPs with different chemical composition (consisting of Co₃O₄, CoO and Co) and with crystallite sizes ranging from 9 to 18 nm were obtained. Furthermore, the preparation of cobalt oxide-based nanocomposites by twin polymerization of 2,2′-spirobi[4H-1,3,2-benzodioxasiline] (3) in the presence of 2b is reported. After treatment of the as-prepared hybrid material by either oxidation or etching, the respective mesoporous carbon/silica (IUPAC type IV isotherms) matrices were obtained. Quenched solid and nonlinear density functional theory calculations gave a surface area of 1040 cm² g⁻¹ for the respective carbon and 336 cm² g⁻¹ for the appropriate silica material. Powder X-ray diffraction measurements confirm the formation of Co₃O₄ NPs in both components. High-angle annular dark field scanning transmission electron microscopy revealed well-distributed particles within the silica matrix, whereas no particles were found in the carbon material. The electrochemical properties of the composite materials have been investigated by cyclic voltammetry. The respective silica material shows five reduction events (Co₃O₄ to CoO, CoO to Co), while no redox potentials occurred for the Co₃O₄ NPs embedded in the carbon matrix.

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Title: Co(II) ethylene glycol carboxylates for Co3O4 nanoparticle and nanocomposite formation
Authors: K. Assim
S. Schulze
M. Pügner
M. Uhlemann
T. Gemming
L. Giebeler
M. Hietschold
T. Lampke
H. Lang
Publication date: 17-02-2017
Publisher: Springer US
Published in: Journal of Materials Science / Issue 11/2017
Print ISSN: 0022-2461
Electronic ISSN: 1573-4803
DOI: https://doi.org/10.1007/s10853-017-0904-1

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