In this study, SrFe12-xNdxO19, where x = 0, 0.1, 0.2, 0.3, 0.4, and 0.5, was prepared using high-energy ball milling. The prepared samples were characterized by X-ray diffraction (XRD). Using the XRD results, a comparative analysis of crystallite sizes of the prepared powders was carried out by different methods (models) such as the Scherrer, Williamson–Hall (W–H), Halder–Wagner (H–W), and size-strain plot (SSP) method. All the studied methods prove that the average nanocrystallite size of the prepared samples increases by increasing the Nd concentration. The H–W and SSP methods are more accurate than the Scherer or W–H methods, suggesting that these methods are more suitable for analyzing the XRD spectra obtained in this study. The specific saturation magnetization (σs), the effective anisotropy constant (Keff), the field of magnetocrystalline anisotropy (Ha), and the field of shape anisotropy (Hd) for SrFe12-xNdxO19 (0 ≤ x ≤ 0.5) powders were calculated. The coercivity (Hc) increases (about 9% at x = 0.4) with an increasing degree of substitution of Fe3+ by Nd3+, which is one of the main parameters for manufacturing permanent magnets.
Nowadays, magnetoelectric nanomaterials are on their way to finding wide applications in biomedicine for various cancer and neurological disease treatment, which is mainly restricted by their relatively high toxicity and complex synthesis. This study for the first time reports novel magnetoelectric nanocomposites of CoxFe3−xO4-BaTiO3 series with tuned magnetic phase structures, which were synthesized via a two-step chemical approach in polyol media. The magnetic CoxFe3−xO4 phases with x = 0.0, 0.5, and 1.0 were obtained by thermal decomposition in triethylene glycol media. The magnetoelectric nanocomposites were synthesized by the decomposition of barium titanate precursors in the presence of a magnetic phase under solvothermal conditions and subsequent annealing at 700 °C. X-ray diffraction revealed the presence of both spinel and perovskite phases after annealing with average crystallite sizes in the range of 9.0–14.5 nm. Transmission electron microscopy data showed two-phase composite nanostructures consisting of ferrites and barium titanate. The presence of interfacial connections between magnetic and ferroelectric phases was confirmed by high-resolution transmission electron microscopy. Magnetization data showed expected ferrimagnetic behavior and σs decrease after the nanocomposite formation. Magnetoelectric coefficient measurements after the annealing showed non-linear change with a maximum of 89 mV/cm*Oe with x = 0.5, 74 mV/cm*Oe with x = 0, and a minimum of 50 mV/cm*Oe with x = 0.0 core composition, that corresponds with the coercive force of the nanocomposites: 240 Oe, 89 Oe and 36 Oe, respectively. The obtained nanocomposites show low toxicity in the whole studied concentration range of 25–400 μg/mL on CT-26 cancer cells. The synthesized nanocomposites show low cytotoxicity and high magnetoelectric effects, therefore they can find wide applications in biomedicine.
Magnetite–gold dumbbell nanoparticles are essential for biomedical applications due to the presence of two surfaces with different chemical natures and the potential combination of magnetic and plasmonic properties. Here, the remote actuation of Fe3O4-Au hybrid particles in a rotating (1 Hz, 7 mT), static (7 mT) or pulsed low-frequency (31 Hz, 175 mT, 30 s pulse/30 s pause) magnetic field was studied. The particles were synthesized by a high-temperature wet chemistry protocol and exhibited superparamagnetic properties with the saturation magnetization of 67.9 ± 3.0 Am2 kg−1. We showcased the nanoparticles’ controlled aggregation in chains (rotating/static magnetic field) in an aqueous solution and their disaggregation when the field was removed. The investigation of nanoparticle uptake by LNCaP and PC-3 cancer cells demonstrated that Fe3O4-Au hybrids mainly escaped endosomes and accumulated in the cytoplasm. A significant fraction of them still responded to a rotating magnetic field, forming short chains. The particles were not toxic to cells at concentrations up to 210 μg (Fe3O4) mL−1. However, cell viability decrease after incubation with the nanoparticles (≥70 μg mL−1) and exposure to a pulsed low-frequency magnetic field was found. We ascribe this effect to mechanically induced cell destruction. Overall, this makes Fe3O4-Au nanostructures promising candidates for intracellular actuation for future magneto-mechanical cancer therapies.
Redox-responsive and magnetic nanomaterials are widely used in tumor treatment separately, and while the application of their combined functionalities is perspective, exactly how such synergistic effects can be implemented is still unclear. This report investigates the internalization dynamics of magnetic redox-responsive nanoparticles (MNP-SS) and their cytotoxicity toward PC-3 and 4T1 cell lines. It is shown that MNP-SS synthesized by covalent grafting of polyethylene glycol (PEG) on the magnetic nanoparticle (MNP) surface via SS-bonds lose their colloidal stability and aggregate fully in a solution containing DTT, and partially in conditioned media, whereas the PEGylated MNP (MNP-PEG) without S-S linker control remains stable under the same conditions. Internalized MNP-SS lose the PEG shell more quickly, causing enhanced magnetic core dissolution and thus increased toxicity. This was confirmed by fluorescence microscopy using MNP-SS dual-labeled by Cy3 via labile disulfide, and Cy5 via a rigid linker. The dyes demonstrated a significant difference in fluorescence dynamics and intensity. Additionally, MNP-SS demonstrate quicker cellular uptake compared to MNP-PEG, as confirmed by TEM analysis. The combination of disulfide bonds, leading to faster dissolution of the iron oxide core, and the high-oxidative potential Fe3+ ions can synergically enhance oxidative stress in comparison with more stable coating without SS-bonds in the case of MNP-PEG. It decreases the cancer cell viability, especially for the 4T1, which is known for being sensitive to ferroptosis-triggering factors. In this work, we have shown the effect of redox-responsive grafting of the MNP surface as a key factor affecting MNP-internalization rate and dissolution with the release of iron ions inside cancer cells. This kind of synergistic effect is described for the first time and can be used not only in combination with drug delivery, but also in treatment of tumors responsive to ferroptosis.
The Ce2Fe14B intermetallic, like Nd2Fe14B, has the tetragonal Nd2Fe14B-type structure (space group P42/mnm), in which Ce ions have a mixed-valence state characterized by the coexistence of trivalent 4f1 and tetravalent 4f0 electron states. Despite the fact that the saturation magnetization, magnetic anisotropy field, and Curie temperature of the Ce2Fe14B intermetallic are substantially lower than those of Nd2Fe14B and Pr2Fe14B, Ce2Fe14B retains the capacity of being able to be used in the manufacturing of rare-earth permanent magnets. Moreover, at low temperatures, the anisotropy field of Се2Fe14B is higher than that of Nd2Fe14B, and Се2Fe14B does not undergo the spin-reorientation transition. In this respect, studies of (Nd, Ce)-Fe-B alloys, which are intended for the improvement of the service characteristics-to-cost ratio, are very relevant. A model and algorithm for calculating the hysteresis loops of uniaxial hard magnetic materials with allowance for the K1 and K2 (K2 > 0 and K1 > 0 and K1 < 0) magnetic anisotropy constants were developed and allowed us to obtain data on their effect on the parameters of hysteresis loops for a wide temperature range (0–300 K). The simulation and analysis of hysteresis loops of the quasi-ternary intermetallics (Nd1−хСех)2Fe14B (х = 0–1) was performed. Results of the simulation indicate that the alloying of the Nd2Fe14B intermetallic with Ce to x = 0.94 (1) does not completely eliminate the negative effect of spin-reorientation phase transition on the residual magnetization of the (Nd1−хCeх)2Fe14B intermetallic and (2) slightly decreases the slope of magnetization reversal curve.
The structural transformations and magnetic property changes of the Nd16.2FebalCo9.9Ga0.5B7.5 (SG1, SG2) and Nd15.0FebalGa2.0B7.3 (SG3) nanocomposite alloys obtained by melt spinning in the as-quenched state and after annealing at a temperature range of 560–650 °C for 30 min were studied. The methods used were X-ray diffraction analysis, magnetic property measurements, TEM studies, X-ray fluorescence analysis and Mössbauer spectroscopy. Amorphous phase and crystalline phase Nd2Fe14B (P42/mnm) were observed in the alloy after melt spinning. The content of the amorphous phase ranged from 20% to 50% and depended on the cooling rate. Annealing of the alloys resulted in amorphous phase crystallization into Nd2Fe14B and led to the increased coercivity of the alloys up to 1840 kA/m (23.1 kOe) at 600 °C annealing for 30 min. The alloy with the maximum coercivity had a grain size of the Nd2Fe14B phase ≈50–70 nm with an Nd-rich phase between grains.