RESUMO
New heterotrinuclear complexes with the general formula [Cu2Ln(H2L)(HL)(NO3)2]·MeOH (Ln = Ho (1), Er (2), H4L = N,N'-bis(2,3-dihydroxybenzylidene)-1,3-diaminopropane) were synthesized using compartmental Schiff base ligand in conjugation with auxiliary ligands. The compounds were characterized by elemental analysis, ATR-FTIR spectroscopy, X-ray diffraction, TG, DSC, TG-FTIR and XRD analysis. The N2O4 salen-type ligand coordinates 3d and 4f metal centers via azomethine nitrogen and phenoxo oxygen atoms, respectively, to form heteropolynuclear complexes having CuO2Ln cores. In the crystals 1 and 2, two terminal Cu(II) ions are penta-coordinated with a distorted square-pyramidal geometry and a LnIII ion with trigonal dodecahedral geometry is coordinated by eight oxygen atoms from [CuII(H2L)(NO3)]- and [CuII(HL)(NO3)]2- units. Compounds 1 and 2 are stable at room temperature. During heating, they decompose in a similar way. In the first decomposition step, they lose solvent molecules. The exothermic decomposition of ligands is connected with emission large amounts of gaseous products e.g., water, nitric oxides, carbon dioxide, carbon monoxide. The final solid products of decomposition 1 and 2 in air are mixtures of CuO and Ho2O3/Er2O3. The measurements of magnetic susceptibilities and field dependent magnetization indicate the ferromagnetic interaction between CuII and HoIII ions 1.
RESUMO
The paper presents the synthesis of a hydroxyapatite/iron oxide composite utilizing the wet chemical method, as well as the comparison of several selected material characteristics. As follows from the literature reports, hydroxyapatite is a common mineral possessing numerous significant properties. Nowadays, there is an increase in the amount of research on possible modifications of this compound. The promising way to improve hydroxyapatite features is its combination with iron oxide. Particularly, there can be two forms that are distinguished, namely Fe3O4 and γ-Fe2O3. These oxides exhibit valuable properties, particularly magnetism. A combination of the mentioned materials leads to multifunctional composite formation with many potential applications, as follows from several studies. However, this area of science is not fully developed. There are still many aspects to be examined. The synthesized composite and its components were analyzed by employing the following methods. The X-ray diffraction analysis revealed formation of hydroxyapatite and Fe2O3 crystalline phases. Moreover, porosimetry proved a larger specific area for the composite sample in comparison with other materials. The results obtained using the SEM method confirmed an external layer of hydroxyapatite and spherical shapes of internal Fe2O3 particles. Furthermore, the X-ray photoelectron spectroscopy data presented characteristic peaks of Fe, Ca, P, and O atoms in all samples. The Fourier Transform Infrared spectra displayed all the specific vibrations typical of the analyzed materials. What is more, the Vibrating Sample Magnetometer method confirmed the paramagnetic nature of the samples. It could be concluded that the synthesized composite has intermediate properties between the components used in the formation process. The results suggest that these composites are superparamagnetic. This type of material architecture would be well suited for biomedical applications.
