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Synthesis and characterization of Fe3O4-HfO2 nanoparticles by magnetization and hyperfine interactions measurements
2020 - MATOS, IZABELA T.; SALES, TATIANE S.; CABRERA-PASCA, GABRIEL; BURIMOVA, ANASTASIA; SAXENA, RAJENDRA N.; PEREIRA, LUCIANO F.; OTUBO, LARISSA; CARBONARI, ARTUR W.
Nanoparticles (NPs) that combine biocompatibility and enhanced physical characteristics for biomedical applications are currently an area of intense scientific research. Hafnium oxide NPs is an innovative approach in the anticancer treatment by radiotherapy due to their low toxicity and enhancement of local dose in the tumor reducing the total radiation dose for the patient [1]. The combination of this amazing property with the excellent magnetic hyperthermia performance of Fe3O4 NPs can produce a promising nanomaterial for cancer therapy. In the present work, we have synthesized NPs samples of Fe3O4 doped with 10%Hf and HfO2 doped with 10% Fe by chemical procedures. The samples had their morphological, structural, and magnetic properties characterized by some results being displayed in Fig. 1. The crystal structure of the samples was characterized by X-ray Diffraction (XRD), whose results present a single phase. Transmission Electron Microscopy (TEM) images show spherical and hexagonal NPs with an average size of 12 nm as displayed in Fig. 2. The magnetic property was investigated by magnetization measurement. The results from the temperature dependence of ZFC-FC magnetization show a large peak in the ZFC curve corresponding to a broad distribution of blocking temperatures as shown in Fig. 1(b). Fortunately, when irradiated with neutrons in a research reactor, the nuclear reaction 180Hf(n,γ)181Hf yields the probe nucleus 181Hf(181Ta) used by the perturbed angular correlations (PAC) technique to measure hyperfine interactions. Both samples show electric quadrupole interaction characteristics of the HfO2 phase indicating that the Fe replaces Hf in HfO2 NPs, but rather than substituting Fe, Hf form HfO2 NPs diluted in Fe3O4 NPs. Moreover, a pure time-dependent magnetic dipole interaction below 300 K was observed for Fe3O4 NPs mixed with 10% of HfO2.
Annealing effect on the structural and local magnetic properties of nickel ferrite nanoparticles studied by hyperfine interaction measurements
2020 - RODRIGUES, PRISCILA S.; MATOS, IZABELA T.; SALES, TATIANE S.; BURIMOVA, ANASTASIA; CABRERA-PASCA, GABRIEL; PEREIRA, LUCIANO F.; SAXENA, RAJENDRA N.; OTUBO, LARISSA; CARBONARI, ARTUR W.
Nickel ferrite in the form of nanoparticles is a technologically important material that can be applied for the production of biosensors, catalysts, drug delivery, and magnetic resonance contrast agents. In this work NiFe O samples comprising spherical nanoparticles of ~6 nm in diameter have been synthesized via a thermal decomposition route. The quality control of the samples was carried out with conventional techniques including X-ray diffraction and transmission electron microscopy. Post-synthesis XRD pattern revealed textured spinel NiFe O . Local magnetic properties were examined with Time Differential Perturbed Angular Correlation (TDPAC) spectroscopy within the 12 - 773K temperature range with In( Cd) probe introduced into the samples at synthesis. Quasi-static magnetic properties were observed (including above room temperature), as expected due to the small time window of TDPAC. The TDPAC results shown in Fig. 1 were analyzed using a model with combined electric quadrupole and magnetic dipole interactions. An expressive dynamic interaction was observed upon heating after synthesis. A theoretical model based on the Brillouin function for different ionic moments was applied to study the evolution of the hyperfine magnetic field with temperature (see Fig. 1-2) and allowed to attribute the magnetic interaction to the probe location at Fe3+ site. Site occupancy and the interplay between magnetic and structural properties are discussed with respect to application perspectives.
Synthesis and characterization of Fe3O4-HfO2 nanoparticles by hyperfine interactions measurements
2021 - SALES, T.S.N.; BURIMOVA, A.; RODRIGUES, P.S.; MATOS, I.T.; CABRERA-PASCA, G.A.; SAXENA, R.N.; PEREIRA, L.F.D.; OTUBO, L.; CARBONARI, A.W.
Nanoparticles (NPs) that combine biocompatibility and enhanced physical characteristics for biomedical applications are currently an area of intense scientific research. Hafnium oxide NPs are an innovative approach in the anticancer treatment by radiotherapy due to their low toxicity and enhancement of local dose in the tumor reducing the total radiation dose for the patient. The combination of this property with the excellent magnetic hyperthermia performance of Fe3O4 NPs can produce a promising nanomaterial for cancer therapy. In this work, we attempted to synthesize nanoscale samples of HfO2 doped with nominal 10 at.% Fe, and Fe3O4 doped with Hf at 10 at.% level using simple chemical routes. The crystal structure of the samples was characterized by X-ray diffraction. The material was irradiated with neutrons in a research reactor, the nuclear reaction 180Hf(n, γ)181Hf yielding the probe nucleus 181Hf(181Ta) used in the perturbed angular correlations experiments to measure hyperfine interactions. Despite their immediate response to the external magnetic field, at local level both samples showed only electric quadrupole interaction typical of the monoclinic hafnia indicating that Fe replaces Hf in HfO2 NPs, but, rather than substituting Fe, Hf enters magnetite in the form of HfO2 clusters. Transmission Electron Microscopy was exploited to study the morphology of these complex systems, as well as to localize hafnia clusters and understand the nature of their coupling to Fe3O4 specks.
High-saturation magnetization in small nanoparticles of Fe3O4 coated with natural oils
2020 - CORRÊA, BRUNO S.; COSTA, MESSIAS S.; CABRERA-PASCA, GABRIEL A.; SENA, CLEIDILANE; PINTO, RAFAEL H.H.; SILVA, ANA P.S.; CARVALHO JUNIOR, RAUL N.; ISHIDA, LINA; RAMON, JONATHAN G.A.; FREITAS, RAFAEL S.; SAIKI, MITIKO; MATOS, IZABELA T.; CORRÊA, EDUARDO L.; CARBONARI, ARTUR W.
The enhancement of nanoparticle’s magnetic properties with a suitable coating is the main tool to increase their potential as an effective candidate for applications in different areas, especially in biomedicine. In the work here reported, Fe3O4 nanoparticles coated with natural oils were synthesized by iron (III) acetylacetonate thermal decomposition and the effects of the coating on the magnetic properties of these particles have been investigated. The oils were extracted from three Amazon fruits seeds: açaí, ucuúba, and bacaba by CO2 supercritical extraction process, and the relative percentage composition of fatty acids were determined by gas chromatography. A systematic study of crystalline, morphological, and magnetic properties revealed a saturation magnetization (Ms) enhancement and high values of the anisotropy constant for Fe3O4 samples when coated with açaí and ucuúba oils, which present a large percentage of saturated total fatty acid. Our results indicate that nanoparticles with sizes smaller than around 5 nm present Ms values as high as that found for bulk Fe3O4 and, consequently, much higher than Ms values for nanoparticles usually coated with oleic acid. The nuclear techniques neutron activation analysis and perturbed angular correlations were used to better characterize the nanoparticles.
Investigation of magnetic and structural properties of CoFe2O4 nanoparticles by measuring hyperfine interactions with 111Cd
2019 - MATOS, I.T.; NASCIMENTO, N.M.; CABRERA-PASCA, G.A.; EFFENBERGER, F.B.; FREITAS, R.S.; CARBONARI, A.W.
Because their ability of magnetic nanoparticles (MNP) to become magnetized when exposed to an external magnetic field, which make them good candidates for biomedical applications [1]. The investigation of the magnetic and structural properties by techniques with atomic resolution, such as those based on hyperfine interactions, is, therefore, greatly useful in the study of MNP. In this work, hyperfine interactions in nanoparticles of CoFe2O4 were investigated by perturbed γ-γ angular correlation (PAC) spectroscopy using 111Cd as probe nuclei in the temperature range from 50 K to 850 K. Samples of CoFe2O4 were prepared by thermal decomposition [2]. Magnetic measurements results show a blocking temperature of 210 K and a superparamagnetic behavior at 300 K. MET measurements show that particles present well-monodispersed spherical shape with average size of 7 nm. XRD results show that samples crystallize in a single phase with the expected spinel structure. PAC spectra were fitted by a model considering two site fractions occupied by the probe nuclei. One were characterized by a single well-defined Larmor frequency with site fraction population of 47%, which was assigned to probe nuclei substituting cation sites in the core region of the particles. The other was characterized by a broad distribution quadrupole frequency with population of 53% corresponding to probe nuclei at distorted cation sites in the shell region of the particles. This assignment agrees with an expected shell/core volume ratio for particles with a diameter of 7 nm. Hyperfine measurements also show that the magnetic hyperfine field (Bhf) is 12.6 T at 10 K in the saturated region and the temperature dependence of Bhf indicate that the transition temperature is around 900 K.
Caracterização em escala atômica de nanopartículas magnéticas de magnetita e ferrita do tipo TMFe2O4 (TM = Co, Ni) para uso em biomedicina pela espectroscopia de correlação angular gama-gama perturbada
2018 - MATOS, IZABELA T. de
Este trabalho descreve, sob um ponto de vista atômico, a investigação das nanopartículas magnéticas (NPMs) de magnetita (Fe3O4) e ferritas do tipo TMFe2O4 (TM = Co, Ni), que são uma classe de materiais estruturados que atualmente tem um grande interesse devido à grande variedade de suas possíveis aplicações tecnológicas e biomédicas, pela Espectroscopia de Correlação Angular γ-γ Perturbada (CAP). Para a produção das NPMs foram utilizadas duas rotas químicas: o método de co-precipitação e o método de decomposição térmica. A co-precipitação apresenta as vantagens de ter temperaturas moderadas e custos relativamente baixos, porém não se consegue ter um controle da distribuição de tamanho das partículas. Por outro lado, a decomposição térmica possibilita uma amostra monodispersa com controle de tamanho e forma, mas este método necessita de reagentes tóxicos, caros e alta temperatura de reação. Para caracterização das amostras foi usada a técnica de Difração de Raio X (DRX) e a morfologia das NPs foi estudada por meio da Microscopia Eletrônica de Transmissão (MET). A partir desta técnica foi possível avaliar a distribuição do tamanho dos grãos, pois algumas características como, elevado valor de magnetização, alta anisotropia e um alto valor de coercividade são propriedades que dependem das nanoestruturas. As propriedades magnéticas foram estudadas localmente a partir da Correlação Angular Perturbada (CAP) que utiliza como sondas núcleos atômicos das medidas, como os núcleos de prova 111In (111Cd), 140La (140Ce) e 181Hf(181Ta). Estas propriedades foram complementadas por medidas de Magnetização.
Production and study of nanoparticles magnetic properties by hyperfine interactions
2017 - NASCIMENTO, N.M.; CORREA, E.L.; BOSCH-SANTOS, B.; MATOS, I.T.; CABRERA-PASCA, G.A.; CARBONARI, A.W.
In the past years nanotechnology was highlighted as a quick growing field, with many applications in science and technology including information storage, drug delivery and medical images, in which gadolinium-based nanoparticles (NPs) have been studied as contrast agent for magnetic resonance image. On the other hand erbium oxide NPs present potential for many applications due to their optical, electrical and photoluminescence properties, and can be used in display monitors, carbon nanotubes for "green" chemistry and in bioimaging, and iron-based NPs have been studied for application in hyperthermia due to its superparamagnetic properties. At the Hyperfine Interactions Laboratory (LIH) NPs are synthesized by thermal decomposition and co-precipitation. Structural characterization is made using X-ray diffraction (XRD) and transmission electron microscopy (TEM) and magnetic properties are studied by magnetization, both at partner laboratories, and perturbed angular correlation (PAC) spectroscopy using 111In(111Cd) as probe nuclei at LIH. PAC spectroscopy is based on the angular correlation between nuclear radiations emitted by radioactive probe nuclei, which is a well-established method in nuclear spectroscopy. Perturbation occurs in this correlation by electromagnetic interactions external to the nucleus when it is inserted in a material, which can provide information on the electronic distribution of the neighborhood. In this work, an important material was investigated by PAC spectroscopy using 111In, which decays to 111Cd by electron capture, as probe nuclei. Results have shown that NPs produced by thermal decomposition present narrow size distribution, with average size of 5 nm. On the other hand, results related to NPs produced by co-precipitation have shown that NPs don’t have a homogeneity in size and shape distribution.
Hyperfine interactions in Pd foils during D/H electrochemical loading
2016 - SILVA, ERIC B. da; CORREIA, JOAO G.; ZOGHBY, MICHEL; GAHL, JOHN; SCHELL, JULIANA; MATOS, IZABELA T. de; RIBEIRO JUNIOR, IBERE S.; CARBONARI, ARTUR W.; HUBLER, GRAHAM K.; VIOLANTE, VITTORIO; THIOYE, MOUSTAPHA; HE, JINGHAO
The Fleischmann and Pons Effect (FPE) is the appearance of anomalous excess heat during electrolytic loading of hydrogen in metal. Although observed well above measurement uncertainties [1] this effect still remains unexplained. Unlike previous studies where hydrogen (H) was pre-loaded before Time Differential Perturbed Angular Correlations (TDPAC) [2,3] was performed, this present work probes, at the nanoscopic scale, palladium (Pd) samples during H and deuterium (D) loading in 0.1M LiOH or LiOD electrolyte. Radioactive 181Hf (181Ta) was implanted at 80 keV (HISKP-Bonn) and experiments were performed at the ISOLDE-CERN SSP laboratories after vacuum annealing to recover implantation defects. An almost “flat” unperturbed PAC – R(t) spectrum was observed, as expected for Hf/Ta atoms at cubic Pd sites with no remaining point defects in their vicinity. Upon D loading the “flat” unperturbed R(t) spectrum changes to a characteristic Gaussian-like EFG distribution, centered near zero EFG, due to the random distribution of D atoms inside the Pd lattice. With increasing D concentration, the central value of the distribution becomes nonzero, thus revealing that the Pd crystalline structure is relaxed from cubic, consistent with the phase diagram for Pd hydrides. The data also shows that, while being an impurity in the system under study, the Hf/Ta atoms do not trap nor significantly interfere with the H/D atoms in the Pd lattice that would bias the present studies. Thus, further experiments aimed at studying the FPE under external excitations are envisaged.
Síntese de nanopartículas de óxido de ferro utilizando óleo de ucuúba
2015 - CORREA, BRUNO S.; SILVA, ANA P.S.; CORDEIRO, RENATO M.; MATOS, IZABELA T.; CORREA, EDUARDO L.; EFFENBERGER, FERNANDO B.; SENA, CLEIDILANE; CARVALHO JUNIOR, RAUL N.; SAIKI, MITIKO; CARBONARI, ARTUR W.
Sintese e caracterização de nanopartículas magnéticas de Fesub(2)Osub(4) recobertas com óleo de açai para aplicações biomédicas
2015 - SILVA, ANA P.S.; CORREA, BRUNO S.; BATISTA, CAMILA R.; PINTO, RAFAEL H.H.; CORDEIRO, RENATO M.; MATOS, IZABELA T.; EFFENBERGER, FERNANDO B.; JUNIOR, RAUL N.C.; SAIKI, MITIKO; SENA, CLEIDILANE; CARBONARI, ARTUR W.