Nanoparticles have experienced increasing interest over the past three decades owing to the development of new synthesis methods and the adaptation of analysis tools with spatial resolutions below one micrometer. Among the different types of nanoparticles developed in recent years (metals, metal oxides, silica, polymers, etc.), significant scientific interest has developed around iron oxide nanoparticles. This review will focus on these magnetic iron oxide nanoparticles. We will first discuss the magnetic properties of iron oxide nanoparticles, then the different methods of synthesis and washing. Finally, we will discuss some functionalization strategies of iron oxide nanoparticles which are developed within our research team.
Chitin and its derivative chitosan are among the most used polysaccharides for biomedical and pharmaceutical applications. Most of the commercially available chitin is obtained from seafood wastes. However, the interest in alternative renewable sources of chitin and chitosan, such as insects, is growing. When new sources are identified, their stability over time has to be evaluated to allow for their commercialization. The aim of this study is to compare the physicochemical properties of chitin extracted from Cicada orni sloughs harvested in three different years (2017, 2019 and 2020) in order to assess the stability of the source and the repeatability of the extraction process. Chitin and its derivative chitosan were characterized by simple techniques such as Fourier transform infrared spectroscopy (FTIR) and X-ray diffraction (XRD). Results suggest that the physicochemical properties of the extracted chitin varied from year to year, and that these differences are not due to the extraction process, but rather to intrinsic differences within the source. We showed that these differences could already be detected by analyzing the raw material (i.e., cicada sloughs) using the above-mentioned simple methods. The chitosan obtained from deacetylation of chitin had a low degree of deacetylation (%). This low degree of deacetylation can be attributed to the deacetylation process, which is probably not appropriate for this source of chitin.
Iron oxide nanoparticles are extensively utilized in various fields, particularly in biomedical applications. For such uses, nanoparticles must meet specific criteria, including precise size, morphology, physico-chemical properties, stability, and biocompatibility. Microwave-assisted co-precipitation offers an efficient method for producing water-soluble nanoparticles. Functionalization with citrate during synthesis is crucial for achieving a stable colloidal solution. This study aims to compare the effectiveness of conventional co-precipitation with microwave-assisted co-precipitation. The synthesized nanoparticles were characterized using TEM, DLS, FTIR, XRD, and magnetic measurements. The findings indicate that the in situ citrate functionalization during synthesis results in stable, non-aggregated nanoparticles.
In this study, two copper(II) complexes, [Cu(C6H8N3S2)2]Cl2 (1) and [Cu(C7H10N3S2)2]Cl2·H2O (2), were synthesized from 2-(thiophen-2-ylmethylene)hydrazine-1-carbothioamide (L1H) and 2-(1-(thiophen-2-yl)ethylidene)hydrazine-1-carbothioamide (L2H) respectively and characterized using various spectroscopic techniques and elemental analyses. The as-prepared complexes were used as single-source precursors for the synthesis of oleylamine-capped (OLA@CuxSy), hexadecylamine-capped (HDA@CuxSy), and dodecylamine-capped (DDA@CuxSy) copper sulphide nanoparticles (NPs) via the thermolysis method at 190 °C and 230 °C and then characterized using powder X-ray diffraction (p-XRD), UV-visible spectroscopy, transmission electron microscopy (TEM), and scanning electron microscopy (SEM). The p-XRD diffraction patterns confirmed the formation of crystalline rhombohedral digenite Cu9S5 with the space group R-3m. The TEM images showed the formation of nanoparticles of various shapes including hexagonal, rectangular, cubic, truncated-triangular, and irregularly shaped Cu9S5 nanomaterials. The SEM results showed aggregates and clusters as well as the presence of pores on the surfaces of nanoparticles synthesized at 190 °C. The UV-visible spectroscopy revealed a general blue shift observed in the absorption band edge of the copper sulphide NPs, as compared to bulk CuxSy, with energy band gaps ranging from 2.52 to 3.00 eV. Energy-dispersive X-ray spectroscopy (EDX) confirmed the elemental composition of the Cu9S5 nanoparticles. The nanoparticles obtained at 190 °C and 230 °C were used as catalysts for the photocatalytic degradation of methylene blue (MB) under UV irradiation. Degradation rates varying from 47.1% to 80.0% were obtained after 90 min of exposure time using only 10 mg of the catalyst, indicating that Cu9S5 nanoparticles have potential in the degradation of organic pollutants (dyes).
Superparamagnetic Iron Oxide Nanoparticles (SPIONs) are widely used in various areas of the biomedical field: for diagnosis (Magnetic Resonance Imaging), for therapeutic applications (hyperthermia, nanovectorization). These applications require a good stability in water and no aggregation of SPIONs, with well-controlled physicochemical and magnetic properties. In this work, SPIONs functionalized by citrate ligands are synthesized in a one-step process with the aim of producing stable water-dispersible nanoparticles with a well-crystallized spinel structure. Microwave technology is implemented to achieve this objective given the ease, speed and reproducibility of the method. For their future use in biomedical applications, the sterilization of these SPIONs are essential by an autoclave treatment. The influence of this treatment on the physicochemical and magnetic properties of the SPIONs is determined by a systematic characterization before and after sterilization by Transmission Electronic Microscopy, Dynamic Light Scattering, X-ray Diffraction, Fourier Transformed Infra-Red, ThermoGravimetric Analysis and magnetic measurements.
We report the synthesis of lead(II) complexes of 2-(thiophen-2-ylmethylene) hydrazine-1-carbothioamide (1) and 2-(1-(thiophen-2-yl) ethylene) hydrazine-1-carbothioamide (2), which were used as single source precursors in hexadecylamine (HDA) and oleylamine (OLA) at 190, 230, and 270°C to synthesize lead(II) sulfide nanoparticles. Optical studies by UV–vis analysis showed a general blue shift in the absorption band edge of the PbS nanoparticles (NPs) with energy bandgaps determined by Tauc’s plots ranging from 2.15 to 3.11 eV. The development of NPs with a variety of morphologies that changed with temperature and precursor type was demonstrated by morphological characterization using scanning electron microscopy and transmission electron microscopy. Cubic, rod-shaped, and nearly spherical-shaped PbS were formed. Powder X-ray diffraction (p-XRD) structural studies revealed the face-centered cubic structure of PbS nanoparticles. The elements contained in the nanoparticles were identified by energy dispersive X-ray spectroscopy (EDX). These results suggest that the size, shape, and optical properties of the synthesized PbS NPs were affected by reaction temperature, capping group, and precursor type. Under UV irradiation, the photocatalytic activity of HDA-capped PbS nanoparticles on the degradation of methylene blue dye ranged from 28.3% to 60.0%, with lead sulfide nanoparticle obtained by thermolysis of complex (1) at 230°C showing the highest photocatalytic efficiency (60.0%).