223 research outputs found

    Dry impregnation in fluidized bed: Drying and calcination effect on nanoparticles dispersion and location in a porous support

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    The synthesis of metal nanoparticles dispersed inside the grains of a porous inorganic support was carried out by ‘‘dry impregnation’’ in a fluidized bed. The principle of this technique consists in the spraying of a solution containing a metal source into a hot fluidized bed of porous particles. The metal source can be of different nature such as metal salts, organometallic precursors or colloidal solutions. The experimental results obtained from iron oxide deposition on a porous silica gel as support, constitute the core of this article but others results concerning the deposition of rhodium from a colloidal suspension containing preformed rhodium nanoparticles are also described. More precisely, this study aims to understand the effect of the bed temperature during the impregnation step, the initial particle porosity and the calcination operating protocol on the metallic nanoparticles dispersion and location in the silica porous particles. The so-obtained products were characterized by various techniques in order to determine their morphology, their surface properties and the dispersion of the nanoparticles inside the support. The results showed that, under the chosen operating conditions, the deposit efficiency is close to 100% and the competition between the drying rate, depending on the process-related variables, and the capillary penetration rate, depending on the physicochemical-related variables, controls the deposit location. A quasi uniform deposit inside the support particles is observed for soft drying. The metal nanoparticles size is controlled by the pore mean diameter of the support as well as the calcination operating protocol

    Synthesis of Supported Catalysts by Dry Impregnation in Fluidized Bed

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    The synthesis of catalytic or not composite materials by dry impregnation in fluidized bed is described. This process can be carried out under mild conditions from solutions of organometallic precursors or colloidal solutions of preformed nanoparticles giving rise to reproducible metallic nanoparticles containing composite materials with a high reproducibility. The adequate choice of the reaction conditions makes possible to deposit uniformly the metal precursor within the porous matrix or on the support surface. When the ratio between the drying time and the capillary penetration time (tsec/tcap) is higher than 10, the impregnation under soft drying conditions leads to a homogeneous deposit inside the pores of the particles of support. The efficiency of the metal deposition is close to 100%, and the size of the formed metal nanoparticles is controlled by the pores diameter. Finally, some of the presented composite materials have been tested as catalysts: iron-based materials were used in carbon-nanotubes synthesis, while Pd and Rh composite materials have been investigated in hydrogenation reactions

    Influence of a transverse static magnetic field on the magnetic hyperthermia properties and high-frequency hysteresis loops of ferromagnetic FeCo nanoparticles

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    The influence of a transverse static magnetic field on the magnetic hyperthermia properties is studied on a system of large-losses ferromagnetic FeCo nanoparticles. The simultaneous measurement of the high-frequency hysteresis loops and of the temperature rise provides an interesting insight into the losses and heating mechanisms. A static magnetic field of only 40 mT is enough to cancel the heating properties of the nanoparticles, a result reproduced using numerical simulations of hysteresis loops. These results cast doubt on the possibility to perform someday magnetic hyperthermia inside a magnetic resonance imaging setup.Comment: 6 pages, 3 figure

    Magnetic anisotropy determination and magnetic hyperthermia properties of small Fe nanoparticles in the superparamagnetic regime

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    We report on the magnetic and hyperthermia properties of iron nanoparticles synthesized by organometallic chemistry. They are 5.5 nm in diameter and display a saturation magnetization close to the bulk one. Magnetic properties are dominated by the contribution of aggregates of nanoparticles with respect to individual isolated nanoparticles. Alternative susceptibility measurements are been performed on a low interacting system obtained after eliminating the aggregates by centrifugation. A quantitative analysis using the Gittleman s model allow a determination of the effective anisotropy Keff = 1.3 * 10^5 J.m^{-3}, more than two times the magnetocristalline value of bulk iron. Hyperthermia measurements are performed on agglomerates of nanoparticles at a magnetic field up to 66 mT and at frequencies in the range 5-300 kHz. Maximum measured SAR is 280 W/g at 300 kHz and 66 mT. Specific absorption rate (SAR) displays a square dependence with the magnetic field below 30 mT but deviates from this power law at higher value. SAR is linear with the applied frequency for mu_0H=19 mT. The deviations from the linear response theory are discussed. A refined estimation of the optimal size of iron nanoparticles for hyperthermia applications is provided using the determined effective anisotropy value

    Magnetoresistance and collective Coulomb blockade in super-lattices of ferromagnetic CoFe nanoparticles

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    We report on transport properties of millimetric super-lattices of CoFe nanoparticles surrounded by organic ligands. R(T)s follow R(T) = R_0.exp(T/T_0)^0.5 with T_0 ranging from 13 to 256 K. At low temperature I(V)s follow I=K[(V-V_T)/V_T]^ksi with ksi ranging 3.5 to 5.2. I(V) superpose on a universal curve when shifted by a voltage proportional to the temperature. Between 1.8 and 10 K a high-field magnetoresistance with large amplitude and a strong voltage-dependence is observed. Its amplitude only depends on the magnetic field/temperature ratio. Its origin is attributed to the presence of paramagnetic states present at the surface or between the nanoparticles. Below 1.8 K, this high-field magnetoresistance abruptly disappears and inverse tunnelling magnetoresistance is observed, the amplitude of which does not exceed 1%. At this low temperature, some samples display in their I(V) characteristics abrupt and hysteretic transitions between the Coulomb blockade regime and the conductive regime. The increase of the current during these transitions can be as high as a factor 30. The electrical noise increases when the sample is near the transition. The application of a magnetic field decreases the voltage at which these transitions occur so magnetic-field induced transitions are also observed. Depending on the applied voltage, the temperature and the amplitude of the magnetic field, the magnetic-field induced transitions are either reversible or irreversible. These abrupt and hysteretic transitions are also observed in resistance-temperature measurements. They could be the soliton avalanches predicted by Sverdlov et al. [Phys. Rev. B 64, 041302 (R), 2001] or could also be interpreted as a true phase transition between a Coulomb glass phase to a liquid phase of electrons

    Magnetic hyperthermia in single-domain monodisperse FeCo nanoparticles: Evidences for Stoner-Wohlfarth behaviour and large losses

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    We report on hyperthermia measurements on a colloidal solution of 15 nm monodisperse FeCo nanoparticles (NPs). Losses as a function of the magnetic field display a sharp increase followed by a plateau, which is what is expected for losses of ferromagnetic single-domain NPs. The frequency dependence of the coercive field is deduced from hyperthermia measurement and is in quantitative agreement with a simple model of non-interacting NPs. The measured losses (1.5 mJ/g) compare to the highest of the literature, though the saturation magnetization of the NPs is well below the bulk one.Comment: 14 pages, 3 figure

    Uniform Ru nanoparticles on N-doped graphene for selective hydrogenation of fatty acids to alcohols

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    [EN] Ruthenium nanoparticles (Ru NPs) supported on reduced-graphene oxide doped with N (NH2-rGO) was synthesized and used for the selective hydrogenation of fatty acids to alcohols, being the hydrogenation of palmitic acid selected as model. Ru was stabilized forming uniform nanometer size particles on N-doped graphene (Ru/NH2-rGO). The resultant catalyst was very selective for the carbonyl reduction giving 93% of the aliphatic alcohol at 99% conversion. The Ru/NH2-rGO catalysts was more active and selective than the corresponding Ru on non-doped graphene (Ru/rGO) or Ru on carbon (Ru/C). Mechanistic studies points to a dual mechanism for H-2 dissociation, i.e. homolytic and heterolytic cleavage exists on the Ru/NH2-rGO, while only the homolytic H-2 dissociation occurs on Ru/rGO. This heterolytic splitting, which activates the carbonyl groups and facilitates the hydrogenation of aliphatic acids, is due to the presence of basic centres next to the Ru atoms. The presence of N atoms also increases the stability of the catalyst, allowing a reuse up to four times. (C) 2019 Elsevier Inc. All rights reserved.The authors thank Institute de Tecnologia Quimica (ITQ), Consejo Superior de Investigaciones Cientificas (CSIC) and Universitat Politecnica de Valencia (UPV) for the facilities and Severo Ochoa excellence programme, "Juan de la Cierva" programme and Primeros Proyectos de Investigacion (PAID-06-18) for financial support. We gratefully acknowledge Prof. A. Corma for his invaluable contribution to this research. We also thank the Electron Microscopy Service of the UPV for TEM facilities, Jose A. Vidal-Moya (ITQ CSIC-UPV) for NMR measurements and J. Gaona and C. Morales for their assistance in catalytic reactions.Martínez-Prieto, LM.; Puche Panadero, M.; Cerezo-Navarrete, C.; Chaudret, B. (2019). Uniform Ru nanoparticles on N-doped graphene for selective hydrogenation of fatty acids to alcohols. Journal of Catalysis. 377:429-437. https://doi.org/10.1016/j.jcat.2019.07.040S42943737

    Про водогосподарський комплекс Криму

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    В статье дается определение понятия "водохозяйственный комплекс региона". Приводятся количественные и качественные характеристики состояния развития этой отрасли в АРК. Делаются выводы и предложения относительно повышения эффективности функционирования отрасли, улучшению качества предоставляемых услуг.У статті дається визначення поняття "водогосподарський комплекс регіону". Приводяться кількісні і якісні характеристики стану розвитку цієї галузі в АРК. Робляться висновки й пропозиції щодо підвищення ефективності функціонування галузі, поліпшенню якості надаваних послуг.There is given the definition of concept "a water complex of the region" in this article. Quantitative are resulted and qualitative behaviors of a condition of development of this area in АRК. The conclusions and proposals concerning increase of efficiency of operation of area, improvement of the quality of rendered services are done

    Tuning complex shapes in Pt(0) nanoparticles : from cubic dendrites to five-fold stars

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    A platinum star performance: Quasi-single-crystalline Pt nanoparticles with peculiar morphologies—cubic dendrites, planar tripods, and fivefold stars—were synthesized in high yield. Shape selectivity was achieved by finely tuning the growth kinetics under a dihydrogen atmosphere
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