Search Results (17)

Little research has focused on using iron nitride as thermoseed particles in magnetic hyperthermia, although magnetite (Fe₃O₄) is commonly used for this purpose. In the present study, we focus on iron nitride, especially ε-Fe_2–3N. ε-Fe_2–3N particles were synthesized from hematite (α-Fe₂O₃) and sodium amide (NaNH₂) under various synthesis conditions, and the heat-generation properties of the particles were investigated to reveal the synthesis conditions that lead to particles with notable heat-generation performance. The particles synthesized at 250 °C for 12 h increased the temperature of an agar phantom by approximately 20 °C under an alternating magnetic field (100 kHz, 125 Oe, 600 s), suggesting that ε-Fe_2–3N particles can be used for magnetic hyperthermia. The analysis results for the particles synthesized under different conditions suggest that the heat-generation properties of ε-Fe_2–3N were affected by several factors, including the nitrogen content, particle size, crystallite size, saturation magnetization, and coercive force. Full article

Tailoring the magnetic properties of iron oxide nanosystems is essential to expanding their biomedical applications. In this study, 34 nm iron oxide nanocubes with two phases consisting of Fe₃O₄ and α-Fe₂O₃ were annealed for 2 h in the presence of O₂, N₂, He, and Ar to tune the respective phase volume fractions and control their magnetic properties. X-ray diffraction and magnetic measurements were carried out post-treatment to evaluate changes in the treated samples compared to the as-prepared samples, showing an enhancement of the α-Fe₂O₃ phase in the samples annealed with O₂ while the others indicated a Fe₃O₄ enhancement. Furthermore, the latter samples indicated enhancements in crystallinity and saturation magnetization, while coercivity enhancements were the most significant in samples annealed with O₂, resulting in the highest specific absorption rates (of up to 1000 W/g) in all the applied fields of 800, 600, and 400 Oe in agar during magnetic hyperthermia measurements. The general enhancement of the specific absorption rate post-annealing underscores the importance of the annealing atmosphere in the enhancement of the magnetic and structural properties of nanostructures. Full article

Here, we present the results of the synthesis, surface modification, and properties analysis of magnetite-based nanoparticles, specifically Co_0.047Fe_2.953O₄ (S1) and Co_0.086Fe_2.914O₄ (S2). These nanoparticles were synthesized using the co-precipitation method at 80 °C for 2 h. They exhibit a single-phase nature and crystallize in a spinel-type structure (space group Fd$\overline{\mathsf{3}}$m). Transmission electron microscopy analysis reveals that the particles are quasi-spherical in shape and approximately 11 nm in size. An observed increase in saturation magnetization, coercivity, remanence, and blocking temperature in S2 compared to S1 can be attributed to an increase in magnetocrystalline anisotropy due to the incorporation of Co ions in the crystal lattice of the parent compound (Fe₃O₄). The heating efficiency of the samples was determined by fitting the Box-Lucas equation to the acquired temperature curves. The calculated Specific Loss Power (SLP) values were 46 W/g and 23 W/g (under H_AC = 200 Oe and f = 252 kHz) for S1 and S2, respectively. Additionally, sample S1 was coated with citric acid (Co_0.047Fe_2.953O₄@CA) and poly(acrylic acid) (Co_0.047Fe_2.953O₄@PAA) to obtain stable colloids for further tests for magnetic hyperthermia applications in cancer therapy. Fits of the Box-Lucas equation provided SLP values of 21 W/g and 34 W/g for CA- and PAA-coated samples, respectively. On the other hand, X-ray photoelectron spectroscopy analysis points to the catalytically active centers Fe²⁺/Fe³⁺ and Co²⁺/Co³⁺ on the particle surface, suggesting possible applications of the samples as heterogeneous self-heating catalysts in advanced oxidation processes under an AC magnetic field. Full article

Tuning and controlling the magnetic properties of nanomaterials is crucial to implement new and reliable technologies based on magnetic hyperthermia, spintronics, or sensors, among others. Despite variations in the alloy composition as well as the realization of several post material fabrication treatments, magnetic heterostructures as ferromagnetic/antiferromagnetic coupled layers have been widely used to modify or generate unidirectional magnetic anisotropies. In this work, a pure electrochemical approach has been used to fabricate core (FM)/shell (AFM) Ni@(NiO,Ni(OH)₂) nanowire arrays, avoiding thermal oxidation procedures incompatible with integrative semiconductor technologies. Besides the morphology and compositional characterization of these core/shell nanowires, their peculiar magnetic properties have been studied by temperature dependent (isothermal) hysteresis loops, thermomagnetic curves and FORC analysis, revealing the existence of two different effects derived from Ni nanowires’ surface oxidation over the magnetic performance of the array. First of all, a magnetic hardening of the nanowires along the parallel direction of the applied magnetic field with respect their long axis (easy magnetization axis) has been found. The increase in coercivity, as an effect of surface oxidation, has been observed to be around 17% (43%) at 300 K (50 K). On the other hand, an increasing exchange bias effect on decreasing temperature has been encountered when field cooling (3T) the oxidized Ni@(NiO,Ni(OH)₂) nanowires below 100 K along their parallel lengths. Full article

Magnetic structures exhibiting large magnetic moments are sought after in theranostic approaches that combine magnetic hyperthermia treatment (MH) and diagnostic magnetic resonance imaging in oncology, since they offer an enhanced magnetic response to an external magnetic field. We report on the synthesized production of a core–shell magnetic structure using two types of magnetite nanoclusters (MNC) based on a magnetite core and polymer shell. This was achieved through an in situ solvothermal process, using, for the first time, 3,4-dihydroxybenzhydrazide (DHBH) and poly[3,4-dihydroxybenzhydrazide] (PDHBH) as stabilizers. Transmission electron microscopy (TEM) analysis showed the formation of spherical MNC, X-ray photoelectronic spectroscopy (XPS) and Fourier transformed infrared (FT-IR) analysis proved the existence of the polymer shell. Magnetization measurement showed saturation magnetization values of 50 emu/g for PDHBH@MNC and 60 emu/g for DHBH@MNC with very low coercive field and remanence, indicating that the MNC are in a superparamagnetic state at room temperature and are thus suitable for biomedical applications. MNCs were investigated in vitro, on human normal (dermal fibroblasts-BJ) and tumor (colon adenocarcinoma-CACO2, and melanoma-A375) cell lines, in view of toxicity, antitumor effectiveness and selectivity upon magnetic hyperthermia. MNCs exhibited good biocompatibility and were internalized by all cell lines (TEM), with minimal ultrastructural changes. By means of flowcytometry apoptosis detection, fluorimetry, spectrophotometry for mitochondrial membrane potential, oxidative stress, ELISA-caspases, and Western blot–p53 pathway, we show that MH efficiently induced apoptosis mostly via the membrane pathway and to a lower extent by the mitochondrial pathway, the latter mainly observed in melanoma. Contrarily, the apoptosis rate was above the toxicity limit in fibroblasts. Due to its coating, PDHBH@MNC showed selective antitumor efficacy and can be further used in theranostics since the PDHBH polymer provides multiple reaction sites for the attachment of therapeutic molecules. Full article

In this work, complex studies of the structure and magnetic properties of SrFe_12−xIn_xO₁₉ powders obtained by the mechanochemical and citrate methods were carried out. The solubility of In in strontium hexaferrite SrFe₁₂O₁₉ at 1200 °C was determined. The structure and properties of the powders were studied using X-ray diffraction analysis, Mössbauer spectroscopy and scanning electron microscopy. Measurements of magnetic properties in magnetic fields up to 1600 kA/m were also performed. Additionally, the hyperthermia effect was investigated. The possibility of controlling the coercivity of the samples in the range from 188.9 kA/m to 22.3 kA/m and saturation magnetization from 63.5 A·m²/kg to 44.2 A·m²/kg with an increase in the degree of In doping was also demonstrated. Investigation of the magnetic hyperthermia of the samples was carried out by temperature measurement with an IR camera when they were introduced into alternating magnetic fields of various frequencies (144, 261 and 508 kHz) and amplitudes (between 11.96 and 19.94 kA/m). According to the study result, there was detected the heating of the SrFe_12−xIn_xO₁₉ sample (x = 1.7). The highest values of magnetic hyperthermia of the sample were observed in a 19.94 kA/m magnetic field and a frequency of 261 kHz. At a concentration of 56.67 g/L, the sample was heated from 23 to 41 °C within 2 min. The parameters SLP (specific loss power) and ILP (intrinsic loss power) were calculated. Full article

The combination of magnetic hyperthermia with chemotherapy is considered a promising strategy in cancer therapy due to the synergy between the high temperatures and the chemotherapeutic effects, which can be further developed for targeted and remote-controlled drug release. In this paper we report a simple, rapid, and reproducible method for the preparation of thermosensitive magnetoliposomes (TsMLs) loaded with doxorubicin (DOX), consisting of a lipidic gel formation from a previously obtained water-in-oil microemulsion with fine aqueous droplets containing magnetic nanoparticles (MNPs) dispersed in an organic solution of thermosensitive lipids (transition temperature of ~43 °C), followed by the gel hydration with an aqueous solution of DOX. The obtained thermosensitive magnetoliposomes (TsMLs) were around 300 nm in diameter and exhibited 40% DOX incorporation efficiency. The most suitable MNPs to incorporate into the liposomal aqueous lumen were Zn ferrites, with a very low coercive field at 300 K (7 kA/m) close to the superparamagnetic regime, exhibiting a maximum absorption rate (SAR) of 1130 W/gFe when dispersed in water and 635 W/gFe when confined inside TsMLs. No toxicity of Zn ferrite MNPs or of TsMLs was noticed against the A459 cancer cell line after 48 h incubation over the tested concentration range. The passive release of DOX from the TsMLs after 48h incubation induced a toxicity starting with a dosage level of 62.5 ug/cm². Below this threshold, the subsequent exposure to an alternating magnetic field (20–30 kA/m, 355 kHz) for 30 min drastically reduced the viability of the A459 cells due to the release of incorporated DOX. Our results strongly suggest that TsMLs represent a viable strategy for anticancer therapies using the magnetic field-controlled release of DOX. Full article

The collective organization of magnetic nanoparticles (MNPs) influences significantly their hyperthermic properties, relevant for their in vitro and in vivo applications. We report a systematic investigation of the effects of the concentration and the static bias direct current (DC) magnetic field superposed over the alternating magnetic field (AMF), both in a parallel and perpendicular configuration, on the specific absorption rate (SAR) by using zinc ferrite MNPs. The nonmonotonic dependence of the SAR on the concentration, with a maximum at very small concentrations (c ≤ 0.1 mgFe/mL), followed by a minimum at 0.25 mgFe/mL, and the second maximum of 3.3 kW/gFe at around 1 mgFe/mL, was explained by the passage of the MNPs from a single particle behavior to a collective one and the role of the dipolar interactions. By superposing a static 10 kA/m bias DC field on the AMF we obtained an increase in the SAR for both parallel and perpendicular orientations, up to 4285 W/g_Fe and 4070 W/g_Fe, respectively. To the best of our knowledge, this is the first experimental proof of a significant enhancement of the SAR produced by a perpendicular DC field. The effect of the DC field to increase the SAR is accompanied by an increase in the hyperthermia coercive field (H_cHyp) for both configurations. No enhancement of the DC fields was noticed for the MNPs immobilized in a solid matrix but the DC field increases the H_cHyp only in the parallel configuration. This translates into a higher SAR value for the perpendicular configuration as compared to the parallel configuration. These results have practical applications for magnetic hyperthermia. Full article

In this work, tetrahydroxyquinone (THQ) was used for the first time to coat iron oxide nanoparticles (IONPs) and to carry out in vitro experiments in magnetic hyperthermia. Synthesis by co-precipitation resulted in spherical IONPs with a core diameter of 13 ± 3 nm and covered by a 0.5 nm thick coat of THQ, which provided them with a reasonably good zeta potential of ζ = −28 ± 2 mV at pH = 7.3, and thus colloidal stability. The magnetic properties of the THQ-coated IONPs are promising: the low coercive field of H_c = 7 Oe, the high magnetic saturation of M_s = 70.5 emu/g and the low blocking temperature of T_b = 273 K indicate superparamagnetic characteristics at room temperature. Additionally, a high specific absorption rate SAR = 135 W/g (at 300 Oe and 530 kHz) was determined. Cell biological experiments using the human cell line HT-29 evidenced negligible cytotoxicity up to 2 mg/mL. Magnetic hyperthermia (MHT) assays demonstrated fast and reliable heating and reduced the metabolic activity of the cells to 42% upon reaching 42 °C within 15 min. The production of ROS by THQ-coated IONPs could not be detected, which may indicate a reduction in the undesired side effects caused by oxidative stress. Considering these good physicochemical and cell biological properties, this ferrofluid is a promising candidate for the initiation of in vivo experiments for cancer treatment by MHT in murine models. Full article

The present work reports the synthesis of a stable aqueous magnetic fluid (AMF) by dispersing double-surfactant-coated Fe₃O₄ magnetic nanoparticles (MNPs) in water using a facile ambient scalable wet chemical route. MNPs do not disperse well in water, resulting in low stability. This was improved by dispersing double-surfactant (oleic acid and sodium oleate)-coated MNPs in water, where cross-linking between the surfactants improves the stability of the AMFs. The stability was probed by rheological measurements and all the AMF samples showed a good long-term stability and stability against a gradient magnetic field. Further, the microwave spin resonance behavior of AMFs was studied in detail by corroborating the experimental results obtained from the ferromagnetic resonance (FMR) technique to theoretical predictions by appropriate fittings. A broad spectrum was perceived for AMFs which indicates strong ferromagnetic characteristics. The resonance field shifted to higher magnetic field values with the decrease in particle size as larger-size MNPs magnetize and demagnetize more easily since their magnetic spins can align in the field direction more definitely. The FMR spectra was fitted to obtain various spin resonance parameters. The asymmetric shapes of the FMR spectra were observed with a decrease in particle sizes, which indicates an increase in relaxation time. The relaxation time increased with a decrease in particle sizes (sample A to D) from 37.2779 ps to 42.8301 ps. Further, a detailed investigation of the structural, morphological, and dc magnetic properties of the AMF samples was performed. Room temperature dc magnetic measurements confirmed the superparamagnetic (SPM) characteristics of the AMF and the M-H plot for each sample was fitted with a Langevin function to obtain the domain magnetization, permeability, and hydrodynamic diameter of the MNPs. The saturation magnetization and coercivity of the AMF samples increased with the increase in dispersed MNPs’ size of the samples. The improvement in the stability and magnetic characteristics makes AMFs suitable candidates for various biomedical applications such as drug delivery, magnetic fluid hyperthermia, and biomedicines. Full article

In this report, the heating efficiencies of γ-Fe₂O₃ and hybrid γ-Fe₂O₃-TiO₂ nanoparticles NPs under an alternating magnetic field (AMF) have been investigated to evaluate their feasible use in magnetic hyperthermia. The NPs were synthesized by a modified sol-gel method and characterized by different techniques. X-ray diffraction (XRD), Mössbauer spectroscopy and electron microscopy analyses confirmed the maghemite (γ-Fe₂O₃) phase, crystallinity, good uniformity and 10 nm core sizes of the as-synthesized composites. SQUID hysteresis loops showed a non-negligible coercive field and remanence suggesting the ferromagnetic behavior of the particles. Heating efficiency measurements showed that both samples display high heating potentials and reached magnetic hyperthermia (42 °C) in relatively short times with shorter time (~3 min) observed for γ-Fe₂O₃ compared to γ-Fe₂O₃-TiO₂. The specific absorption rate (SAR) values calculated for γ-Fe₂O₃ (up to 90 W/g) are higher than that for γ-Fe₂O₃-TiO₂ (~40 W/g)_, confirming better heating efficiency for γ-Fe₂O₃ NPs. The intrinsic loss power (ILP) values of 1.57 nHm²/kg and 0.64 nHm²/kg obtained for both nanocomposites are in the range reported for commercial ferrofluids (0.2–3.1 nHm²/kg). Finally, the heating mechanism responsible for NP heat dissipation is explained concluding that both Neel and Brownian relaxations are contributing to heat production. Overall, the obtained high heating efficiencies suggest that the fabricated nanocomposites hold a great potential to be utilized in a wide spectrum of applications, particularly in magnetic photothermal hyperthermia treatments. Full article

Today, magnetic hyperthermia constitutes a complementary way to cancer treatment. This article reports a promising aspect of magnetic hyperthermia addressing superparamagnetic and highly Fe/Au core-shell nanoparticles. Those nanoparticles were prepared using a wet chemical approach at room temperature. We found that the as-synthesized core shells assembled with spherical morphology, including face-centered-cubic Fe cores coated and Au shells. The high-resolution transmission microscope images (HRTEM) revealed the formation of Fe/Au core/shell nanoparticles. The magnetic properties of the samples showed hysteresis loops with coercivity (HC) close to zero, revealing superparamagnetic-like behavior at room temperature. The saturation magnetization (MS) has the value of 165 emu/g for the as-synthesized sample with a Fe:Au ratio of 2:1. We also studied the feasibility of those core-shell particles for magnetic hyperthermia using different frequencies and different applied alternating magnetic fields. The Fe/Au core-shell nanoparticles achieved a specific absorption rate of 50 W/g under applied alternating magnetic field with amplitude 400 Oe and 304 kHz frequency. Based on our findings, the samples can be used as a promising candidate for magnetic hyperthermia for cancer therapy. Full article

Magnetic nanoparticles are increasingly employed in biomedical applications such as disease detection and tumor treatment. To ensure a safe and efficient operation of these applications, a noninvasive and accurate characterization of the particles is required. In this work, a magnetic characterization technique is presented in which the particles are excited by specific pulsed time-varying magnetic fields. This way, we can selectively excite nanoparticles of a given size so that the resulting measurement gives direct information on the size distribution without the need for any a priori assumptions or complex postprocessing procedures to decompose the measurement signal. This contrasts state-of-the-art magnetic characterization techniques. The possibility to selectively excite certain particle types opens up perspectives in “multicolor” particle imaging, where different particle types need to be imaged independently within one sample. Moreover, the presented methodology allows one to simultaneously determine the size-dependent coercivity of the particles. This is not only a valuable structure–property relation from a fundamental point of view, it is also practically relevant to optimize applications like magnetic particle hyperthermia. We numerically demonstrate that the novel characterization technique can accurately reconstruct several particle size distributions and is able to retrieve the coercivity–size relation of the particles. The developed technique advances current magnetic nanoparticle characterization possibilities and opens up exciting pathways for biomedical applications and particle imaging procedures. Full article

Spinel ferrite nanoparticles represent a class of magnetic nanoparticles (MNPs) with enormous potential in magnetic hyperthermia. In this study, we investigated the magnetic and heating properties of spinel soft NiFe₂O₄, MnFe₂O₄, and hard CoFe₂O₄ MNPs of comparable sizes (12–14 nm) synthesized by the polyol method. Similar to the hard ferrite, which predominantly is ferromagnetic at room temperature, the soft ferrite MNPs display a non-negligible coercivity (9–11 kA/m) arising from the strong interparticle interactions. The heating capabilities of ferrite MNPs were evaluated in aqueous media at concentrations between 4 and 1 mg/mL under alternating magnetic fields (AMF) amplitude from 5 to 65 kA/m at a constant frequency of 355 kHz. The hyperthermia data revealed that the SAR values deviate from the quadratic dependence on the AMF amplitude in all three cases in disagreement with the Linear Response Theory. Instead, the SAR values display a sigmoidal dependence on the AMF amplitude, with a maximum heating performance measured for the cobalt ferrites (1780 W/g_Fe+Co), followed by the manganese ferrites (835 W/g_Fe+Mn), while the nickel ferrites (540 W/g_Fe+Ni) present the lowest values of SAR. The heating performances of the ferrites are in agreement with their values of coercivity and saturation magnetization. Full article

Magnetic iron oxides have been used in biomedical applications, such as contrast agents for magnetic resonance imaging, carriers for controlled drug delivery and immunoassays, or magnetic hyperthermia for the past 40 years. Our aim is to investigate the effect of pressure and temperature on the structural, thermal, and magnetic properties of iron oxides prepared by hydrothermal synthesis at temperatures of 100–200 °C and pressures of 20–1000 bar. It has been found that pressure influences the type of iron oxide crystalline phase. Thus, the results obtained by Mössbauer characterization are in excellent agreement with X-ray diffraction and optical microscopy characterization, showing that, for lower pressure values (<100 bar), hematite is formed, while, at pressures >100 bar, the major crystalline phase is goethite. In addition, thermal analysis results are consistent with particle size analysis by X-ray diffraction, confirming the crystallization of the synthesized iron oxides. One order of magnitude higher magnetization has been obtained for sample synthesized at 1000 bar. The same sample provides after annealing treatment, the highest amount of good quality magnetite leading to a magnetization at saturation of 30 emu/g and a coercive field of 1000 Oe at 10 K and 450 Oe at 300 K, convenient for various applications. Full article