Design, construction and evaluation of a 3D printed electrochemical flow cell for the synthesis of magnetite nanoparticles

A 3D-printed prototype of an electrochemical flow cell for the synthesis of superparamagnetic magnetite nanoparticles of medium size between 15 and 30 nm was constructed and its performance was evaluated. The cell consists of a series of rectangular channels in a parallel electrode arrangement. Electrolyte flows through the channels as the electric current is supplied to the system and a combination of electrochemical and chemical reactions create the appropriate conditions for magnetite precipitation. Different electric configurations were evaluated and both energy and production efficiencies were calculated to determine the best configuration. Different flow and current values were also investigated, and all the materials were analyzed by X-ray diffraction, transmission electron microscopy, Mossbauer spectroscopy and magnetization curve measurements to determine their effect on particle morphology, composition and magnetic behavior. The best results were obtained for a parallel monopolar configuration, with 100 mA (3 mA cm−2) passing in each two electrodes and a flow value of 30 mL min−1, yielding an energy efficiency of 5.9 kJ g−1 and a production rate of 12.1 mg min−1, approximately 6 times higher than the 100 mL standard cell previously used. Magnetic saturation was 77.3 emu g−1, slightly lower than the bulk material (92–100 emu g−1)The authors gratefully acknowledge the scholarship for doctoral studies of Gerardo Ivan Lozano Gutierrez granted by the National Council of Science and Technology of Mexico (CONACyT). The authors are also grateful to the Ministry of Economy and Competitiveness for the project MAT2015-67557-C2-2-P. Support for a sabbatical leave for NCS from the National Council of Science and Technology of Mexico and Exportadora de Postes S.A. de C.V. are greatly appreciate

Novel, simple, and environmentally safe method for wastewater pollutant removal

In this work, a new methodology has been developed for the elimination of cobalt, nickel and a mixture of both metals from synthetic wastewater in a continuous way. This methodology consists of the electrochemical formation of ferrites of these metals through the oxidation of iron sheets and the reduction of water. Two critical process parameters, current densities and initial pollutant concentration, were analysed. An initial batch prototype resulted in efficiencies on the order of 98% under conditions of applied densities of 50 mA/cm2 and concentrations of both metals of until 100 ppm of the ions. The obtained particles have been characterized by X-ray diffraction to determine the formation of ferrites without the appearance of secondary phases. The formed particle sizes are approximately 30 nm, with hemispherical or flower-like shapes. A flow system prototype was designed for the recirculation of the solution with 100 ppm of both contaminating metals, obtaining approximately 90% recovery with an easy magnetic harvesting. © 2021 The Author

Self-affine fractal vapour-deposited gold surfaces characterization by scanning tunnelling microscopy

The morphological evolution of the surfaces of gold deposits grown from the vapour on smooth glass under nonequilibrium conditions and incident angle near substrate normal is studied at the nanometer level by scanning tunnelling microscopy. For an average film thickness equal to or greater than 500 nm, the interface thickness (ξ) reaches a steady state. Under these conditions, ξ depends on the scan length (L) as ξ ∝ Lα with α = 0.35 ± 0.05 for L > ds, where ds is the columnar size, and α = 0.89 ± 0.05 for L s. These results indicate that the growing surface spontaneously reaches a steady state and it can be described as a self-affine fractal. The value of α for L > ds agrees with the prediction of ballistic deposition models without restructuring, whereas that for L s exceeds the prediction of ballistic models including restructuring.Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas (INIFTA)Facultad de Ciencias Exacta

Self-affine fractal electrodeposited gold surfaces: Characterization by scanning tunneling microscopy

The morphological evolution of columnar gold electrodeposits grown at 100 nm s −1 by electroreducing a gold oxide layer on a gold cathode has been studied at a nanometer level by scanning tunneling microscopy. The interface thickness (ξ) depends on the scan length (L) as ξ∝ L α with α=0.49±0.07 for L > ds, where ds is the average top columnar size, and α=0.90±0.07 for L s. These results prove that the growing surface can be described as a self-affine fractal for length scales greater than the columnar size. Conversely, the columnar surface approaches the behavior of an Euclidean surface.Instituto de Investigaciones Fisicoquímicas Teóricas y AplicadasFacultad de Ciencias Exacta

Self-affine fractal electrodeposited gold surfaces: Characterization by scanning tunneling microscopy

The morphological evolution of columnar gold electrodeposits grown at 100 nm s −1 by electroreducing a gold oxide layer on a gold cathode has been studied at a nanometer level by scanning tunneling microscopy. The interface thickness (ξ) depends on the scan length (L) as ξ∝ L α with α=0.49±0.07 for L > ds, where ds is the average top columnar size, and α=0.90±0.07 for L s. These results prove that the growing surface can be described as a self-affine fractal for length scales greater than the columnar size. Conversely, the columnar surface approaches the behavior of an Euclidean surface.Instituto de Investigaciones Fisicoquímicas Teóricas y AplicadasFacultad de Ciencias Exacta

Electrochemical synthesis and magnetic properties of MFe_2O_4 (M = Fe, Mn, Co, Ni) nanoparticles for potential biomedical applications

In this study, we evaluate the magnetic properties and cytotoxic effect of magnetic nanoparticles (MNPs) based on magnetite and Mn, Co and Ni ferrites, obtained by electrochemical synthesis. These nanoparticles have almost spherical shape and an mode size of 9 +/- 1 nm. The electrochemical synthesis produces a single crystallographic phase with a spinel-like structure in all cases. Magnetization saturation at room temperature varies with the composition of the ferrites from M_S (Fe_3O_4) > M_S (MnFe_2O_4) > M_S (CoFe_2O_4) > M_S (NiFe_2O_4). Ferrite MNPs present low magnetic remanence indicating a superparamagnetic-like response at room temperature. However, the different values of magnetic anisotropy and size produce variations in the values of coercivity and susceptibility of the ferrite MNPs. The cytotoxicity of the different ferrites was evaluated by internalizing MNP in HeLa cancer cells. Although magnetite and Mn ferrite present low toxicity for all the concentrations studied, significant cytotoxic effect were observed when incubating the cells with high concentration of Co and Ni ferrites

Cation distribution of cobalt ferrite electrosynthesized nanoparticles: A methodological comparison

Final publication at http://doi.org/10.1016/j.jallcom.2017.12.342, © 2017 Elsevier B.V.The present work seeks to analyse the structural and magnetic properties of cobalt ferrite nanoparticles obtained by electrochemical synthesis by high-resolution transmission electronic microscopy (HRTEM), X-ray absorption spectroscopy (XAS), Mössbauer spectroscopy (MS), neutron diffraction (ND) and SQUID magnetometer. The cationic distribution is analyzed by different techniques. The inversion degree determined by the most accurate measurements was 0.73(1), and the formula for the nanoparticles therefore was (↑Co 0.27 Fe 0.73 )[↓Co 0.73 Fe 1.27 ]O 4 . The magnetic moment found from DC and Mössbauer spectroscopy measurements was 3.8(3) μB, and the coercivity was 7870 Oe at 100 K.This work is supported by the MINECO/FEDER Project MAT2015-67557-C2-2-

Comparison of different methodologies for obtaining nickel nanoferrites

Nickel nanoferrites were obtained by means of four different synthetic wet-routes: co-precipitation (CP), sonochemistry (SC), sonoelectrochemistry (SE) and electrochemistry (E). The influence of the synthesis method on the structural and magnetic properties of nickel ferrite nanoparticles is studied. Although similar experimental conditions such as temperature, pH and time of synthesis were used, a strong dependence of composition and microstructure on the synthesis procedure is found, as electron microscopy, X-ray diffraction and Mössbauer spectroscopy studies reveal. Whereas by means of the CP and SC methods particles of a small size around 5–10 nm, respectively, and composed by different phases are obtained, the electrochemical routes (E and SE) allow obtaining monodisperse nanoparticles, with sizes ranging from 30 to 40 nm, and very close to stoichiometry. Magnetic characterization evidences a superparamagnetic behavior for samples obtained by CP and SC methods, whereas the electrochemical route leads to ferromagnetic ferrite nanoparticles

Highly efficient t2 cobalt ferrite nanoparticles vectorized for internalization in cancer cells

Uniform cobalt ferrite nanoparticles have been synthesized using an electrochemical synthesis method in aqueous media. Their colloidal, magnetic, and relaxometric properties have been analyzed. The novelty of this synthesis relies on the use of iron and cobalt foils as precursors, which assures the reproducibility of the iron and cobalt ratio in the structure. A stable and biocompatible targeting conjugate nanoparticle-folic acid (NP-FA) was developed that was capable of targeting FA receptor positivity in HeLa (human cervical cancer) cancer cells. The biocompatibility of NP-FA was assessed in vitro in HeLa cells using the MTT assay, and morphological analysis of the cytoskeleton was performed. A high level of NP-FA binding to HeLa cells was confirmed through qualitative in vitro targeting studies. A value of 479 Fe+Co mM-1s-1 of transverse relaxivity (r2 ) was obtained in colloidal suspension. In addition, in vitro analysis in HeLa cells also showed an important effect in negative T2 contrast. Therefore, the results show that NP-FA can be a potential biomaterial for use in bio medical trials, especially as a contrast agent in magnetic resonance imaging (MRI)

Self-affine fractal vapour-deposited gold surfaces characterization by scanning tunnelling microscopy

The morphological evolution of the surfaces of gold deposits grown from the vapour on smooth glass under nonequilibrium conditions and incident angle near substrate normal is studied at the nanometer level by scanning tunnelling microscopy. For an average film thickness equal to or greater than 500 nm, the interface thickness (ξ) reaches a steady state. Under these conditions, ξ depends on the scan length (L) as ξ ∝ Lα with α = 0.35 ± 0.05 for L > ds, where ds is the columnar size, and α = 0.89 ± 0.05 for L s. These results indicate that the growing surface spontaneously reaches a steady state and it can be described as a self-affine fractal. The value of α for L > ds agrees with the prediction of ballistic deposition models without restructuring, whereas that for L s exceeds the prediction of ballistic models including restructuring.Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas (INIFTA)Facultad de Ciencias Exacta