Thermal decomposition and reducibility of silica-supported precursors of Cu,Fe and Cu–Fe nanoparticles

Journal of Thermal Analysis and Calorimetry - Poly(butylene succinate) (PBS) nanocomposites filled with nanoprecipitated calcium carbonate (NPCC) were prepared via melt blending. The hybrid...     

Adsorption and Vibration of O Atoms on Fe Low-index and Fe （211） High-index Surfaces

IntroductionThe interaction of oxygen with iron in lowcoverageregimes is considered to be an important step in the for-mation of oxides in corrosion science and in Fisher-Tro-psch process for the synthesis of ammonia over the het-erogeneous catalysts[1]. …     

Iodo Derivatives of Bimetallic Fe—Pd and Fe—Pt Complexes. Crystal Structures of

Summary.  Iodo derivatives of diphosphine-bridged heterobimetallic Fe—Pd and Fe—Pt complexeshave been prepared in which an alkoxysilyl ligand bridges the two metals in a μ₂−η²-SiO manner. In the course of their synthesis by halide exchange from (dppx = dppm (Ph₂ PCH₂ PPh₂) or dppa (Ph₂PNHPPh₂); M = Pd or Pt), loss of the alkoxysilyl ligand occurred resulting in the formation of complexes in which a bridging iodide has replaced, as a 3e⁻-donor, the bridging alkoxysilyl ligand. These complexes of formula (M = Pd, Pt are better prepared by reaction of with [MI₂(cod)]. The crystal structures of (2a), (2b), and  · CH₂Cl₂ (3b · CH₂Cl₂) have been determined by X-ray diffraction. Received January 24, 2001. Accepted February 12, 2001     

Kinetics and Mechanism of Dechlorination of o-Chlorophenol by Nanoscale Pd／Fe

IntroductionTherehasbeenagrowinginterestintheuseofzero valentironforthetreatmentofchlorinatedor ganiccompounds(COCs)inwaterandgroundwater .Thestudieshavebeenfocusedonsuchcompoundsascarbontetrachloride ,trichloroethene ,pesticidesandtherelatedcompounds[1— 7] .Whenironisincontactwithalessreductivemetalsuchaspalladiumwhosecomplexhasbeenusedtohydrogenatenitroben zene[8] ,themetalcouplecanformgalvaniccells .ThisledtothediscoveryofaPd/Febimetalliccomplexofwhichpalladiumservesasacatalystandironasa…     

Syntheses and Structures of Heterometallic Fe–Ta Chalcogenido Clusters

Two Fe–Ta containing sulfido complexes were prepared by the reaction of the metal halide salts with bis-trimethylsilylsulfide in the presence of PMe₃. The complexes demonstrate that coordination chemistry with iron sulfides can give access to a range of heterometallic complexes. In [Cl(Me₃P)Ta( ₂-S)₂( ₃-S)Fe(PMe₃)₂]₂ the two [Cl(Me₃P)Ta] units are arranged around one central Fe₂( ₂-S)₂ unit. In [(Me₃P)₄(MeCN)₂Fe^II]²⁺[(Me₃P)₂Ta^IVFe^II ₃( ₃-S)₄Br₄]^2– a [TaFe₃S₄]²⁺ cuboidal arrangement was observed. The complex salt forms a polymeric structure in the solid-state with weak H-bonds between the ions. The [(Me₃P)₂Ta^IVFe^II ₃( ₃-S)₄Br₄]^2– ion was characterised by magnetic measurements showing strong antiferromagnetic interactions between the metal centres.     

Evaluation of stability of silica-supported Fe–Pd and Fe–Pt nanoparticles in aerobic conditions using thermal analysis

The applications of zerovalent iron nanoparticles (nZVI) exploit their high reactivity which decreases due to oxidation in aerobic conditions during manufacture, application, and storage. In this study, we present the new procedure for estimation of the nZVI stability to oxidation in air. The procedure is suitable for characterization of the novel materials based on the supported nZVI. Nanoscale particles were synthesized inside porous silica supports by incipient wetness impregnation with the metal precursor solutions followed by thermal treatment. The TG–DTA studies revealed the decomposition temperature of the supported precursors, as well as the interaction of Fe and precious metal precursors, which resulted in the formation of alloy nanoparticles. Characterization of the samples by XRD confirmed the formation of the nanoparticles of the metallic Pd, Pt, and Fe phases supported on SiO₂ carriers, as well as the formation of solid solutions based on the structure of precious metals. The new procedure for estimation of the nZVI stability included (1) TPR with hydrogen up to 400–425 °C followed by isothermal reduction at these temperatures; (2) in situ reoxidation with oxygen at room temperature. The samples were reduced “as obtained” and after in situ reoxidation. The results of the TPR studies exhibited that introduction of both Pd and Pt protected the Fe nanoparticles from oxidation with oxygen and air at ambient conditions.     

Preparation and Characterization of Fe/Al2O3 Nanocomposites

IntroductionAl2O3ceramic objects have a wide scope of appli-cations because of their high hardness, high intensity,low density, and superior chemical stability, whereasmetals are widely used for their excellent propertiessuch as good ductibility, electric…     

Formation,Phase, and Elemental Composition of Micro- and Nano-Dimensional Particles of the Fe–Ti System

X-ray fluorescence, X-ray phase analysis, and transmission Mössbauer and NGR spectrometry are used to study the formation, phase, and elemental composition of Fe–Ti particles. The interaction between Fe(III) ions and dispersed titanium in an aqueous solution containing chloride ions and HF is studied. It is shown that the resulting Fe–Ti samples are a set of core–shell microparticles with titanium cores coated with micro- and nanosized α-Fe nucleation centers with the thinness outer layer of iron(III) oxide characterized by a developed surface.     

Formation of active phases of Fe/C,Cr/C and Fe–Cr/C catalysts in oxidative dehydrogenation of ethane

The oxidative dehydrogenation of ethane into ethylene using CO₂ as an oxidant at temperatures of 650–750 °C was carried out over Fe/C, Cr/C and Fe–Cr/C catalysts deposited on a carbon support. Before and after the reaction the catalysts were investigated by X-ray powder diffraction (XRD), in situ magnetometry and transmission electron microscopy methods. The correlation between activity of Fe/C, Cr/C and Fe–Cr/C catalytic systems and their phase composition was established.     

Thermal Treatments of Fe—Mn Alkoxide of Glycerol: Infrared absorption and emission spectroscopy

Synthetic Fe—Mn alkoxide of glycerol samples are submitted to controlled heating conditions and examined by IR absorption spectroscopy. On the other hand, the same sample is studied by infrared emission spectroscopy (IRES), upon heating in situ from 100 to 600°C. The spectral techniques employed in this contribution, especially IRES, show that as a result of the thermal treatments ferromagnetic oxides (manganese ferrite) are formed between 350 and 400°C. Some further spectral changes are seen at higher temperatures.This revised version was published online in November 2005 with corrections to the Cover Date.     

Characterization and application of the Fe(II) and α-ketoglutarate dependent hydroxylase FrbJ

The Fe(II) and α-ketoglutarate-dependent hydroxylase FrbJ was previously demonstrated to utilize FR-900098 synthesizing a second phosphonate FR-33289. Here we assessed its ability to hydroxylate other possible substrates, generating a library of potential antimalarial compounds. Through a series of bioassays and in vitro experiments, we identified two new antimalarials.     

Effect of hydrogen reduction temperature on the microstructure and magnetic properties of Fe–Ni powders

The effect of hydrogen reduction temperature on the properties of Fe–Ni powders was described. The mixed powders of Fe-oxide and NiO were prepared by chemical solution mixing of nitrates powders and calcination at 350 °C for 2 h in air. The calcined powders formed small agglomeration with an average particle size of 100 nm. The microstructure and magnetic properties were investigated by using X-ray diffractometry, thermogravimetry, differential thermal analyzer, and vibrating sample magnetometer. Microstructure and thermal analysis revealed that the Fe-oxide and NiO phase were changed to FeNi₃ phase in the temperature range of 245–310 °C, and by heat-up to 690 °C the FeNi₃ phase was transformed to γ-FeNi phase. The reduced powder at 350 °C showed saturation magnetization of 76.3 emu/g and coercivity of 205.5 Oe, while the reduced powders at 690 °C exhibited saturation magnetization of 84.0 emu/g and coercivity of 14.0 Oe. The change of magnetic properties was discussed by the observed microstructural features.

     

Electrochemical and microgravimetric characterization of magnetron-sputtered Fe–Cr–Ni–Ta and Fe–Cr–Ni alloy films in neutral and strongly acidic media

The Fe–Cr–Ni and Fe–Cr–Ni–Ta alloy films were deposited on quartz substrates by magnetron-sputtering using targets of AISI 316 stainless steel and in combination with pure tantalum. The conventional melting of the Fe–Cr–Ni–Ta alloy formed is virtually impossible because the melting point of tantalum is higher than the boiling points of the other components. Elemental content of the films was determined by XPS analysis. Corrosion behaviour of both alloy films was studied in 5% NaCl and 10 M HCl by electrochemical quartz crystal microgravimetry (EQCM), electrochemical impedance spectroscopy (EIS) and dc-voltammetry. The corrosion resistance of Fe–Cr–Ni–Ta appeared to be significantly higher than that of Fe–Cr–Ni in both neutral (5% NaCl) and strongly acidic (10 M HCl) media. The Fe–Cr–Ni–Ta specimen exhibited an extremely high corrosion resistance in 10 M HCl, where the corrosion rates were about one order of magnitude lower than those of Fe–Cr–Ni in neutral solution. EQCM measurements in NaCl solution indicated accumulation of corrosion products on the Fe–Cr–Ni–Ta surface, which was evident from a distinctive increase in electrode mass. By contrast, the mass of the tantalum-free alloy film decreased with a constant rate, which indicated alloy dissolution to prevail. The corrosion current calculated from the mass decrease was in good agreement with that derived from voltammetric measurements. The EQCM data showed that the corrosion resistance of the Fe–Cr–Ni–Ta alloy film in 10 M HCl was about two orders of magnitude higher than that of the Fe–Cr–Ni.     

Synthesis and Crystal Structure of a Heteronuclear Fe–Ru Silyl Complex*

The reaction of the iron metalate [Fe{Si(OMe)₃}(CO)₃(dppm-P)]⁻ (1b) with [Ru(CO)₃Cl(μ-Cl)]₂ afforded the heterodinuclear complex [(OC)₃{(MeO)₃Si}Fe(μ-dppm)Ru(CO)₃Cl)] (Fe–Ru) (3) in which a long Fe–Ru separation of 2.956(1) ? has been crystallographically evidenced. It was shown by density functional theory (DFT) calculations to correspond to the minimum-energy structure. Upon treatment of the corresponding hydrido complex [HFe{Si(OMe)₃}(CO)₃(dppm-P)] (1a) with [Ru(CO)₃Cl(μ-Cl)]₂, the chloride-bridged tetranuclear hydrido complex [(OC)₃{(MeO)₃Si}Fe(H)(μ-dppm)Ru(CO)₂Cl(μ-Cl)]₂ (4) was formed in which the Fe and Ru centers are only linked via bridging dppm ligands. Electronic supplementary material  The online version of this article (doi:) contains supplementary material, which is available to authorized users.

Influence of Fe concentration on the properties of the electrodeposited Zn–Fe coatings

Electrodeposition of Zn–Fe alloys on a copper substrate from a sulfate bath with different Fe²⁺ concentration (0.05, 0.10 and 0.20 mol L^?1) at room temperature was investigated using cyclic voltammetry. The influence of the Fe²⁺ content in the plating bath on the surface morphology, structural and magnetic properties of the coatings were characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), X-ray diffraction (XRD) and Vibrating Sample Magnetometer (VSM). The results show that the morphology of Zn–Fe films changes with different Fe²⁺ concentration. The EDS analysis demonstrated that the Fe content of the coatings increased with increasing the Fe concentration in the bath. XRD measurements shows the presence of ?Zn (hcp), δ1ZnFe (hcp) and the ΓZnFe (bcc) phases with a (101) preferential orientation in all the electrodeposited films. The magnetic analysis of Zn–Fe films indicated that the saturation magnetization was largely enhanced in comparison to pure Zn, especially with 0.2 at. % Fe, while the coercivity decreased.     

Fe³⁺-immobilized nanoparticle-modified capillary for capillary electrophoretic separation of phosphoproteins and non-phosphoproteins

A fused-silica capillary modified with Fe3?-immobilized magnetic nanoparticles (Fe3?-IMAN) has been investigated for the capillary electrophoretic (CE) separation of phosphoproteins and non-phosphoproteins. The Fe3?-IMAN capillary was achieved by covalently immobilising epoxy-based magnetic silica nanoparticles (160?nm) on the prederivatized 3-aminopropyl-trimethoxysilane (APTMS) fused-silica capillary (75?μm id), followed by disodium iminodiacetate and Fe3?. The buildup process was examined by measuring the streaming potentials of the bare capillary, APTMS capillary, epoxy-based nanoparticle capillary and Fe3?-IMAN capillary by varying the buffer pH. An inverted fluorescence microscope was used to determine the surface features of the Fe3?-IMAN capillary derivatized with morin. Further experimental results confirmed that Fe3?-IMAN bonded on the inner wall of the APTMS capillary could provide sufficient solute-bonded phase interactions to allow for the CE separation of phosphoproteins and non-phosphoproteins at concentration levels down to 50?μg/mL. The highest number of theoretical plates obtained was about 233,000/m, and the relative standard deviation (RSD) for migration times was <2.57% for eight consecutive runs, respectively. Additionally, the Fe3?-IMAN modifing method was also applied to the analyses of bovine milk proteins. With simplicity, high resolving power, and high repeatability, the proposed method has shown great potential for phosphoproteomics applications.     

Synthesis of L10 Fe–Pd films by electrodeposition and thermal annealing

Fe–Pd alloy films have been prepared by electrochemical deposition from an alkaline electrolyte containing Fe sulfate, Pd chloride and 5-sulfosalicylic acid onto polycrystalline titanium substrates. The as-deposited films were nanocrystalline and magnetically soft (coercivity ∼ 25 Oe). L1₀ Fe–Pd films with a (1 1 1) preferred orientation were obtained by post-deposition thermal annealing of films with composition about 37 at% Fe in an (Ar + 5% H₂) gas flow at 500 °C. Such films exhibit hard magnetic properties, with a coercivity up to 1880 Oe, and a slightly anisotropic magnetic response, with a larger in-plane remanence. Preliminary magnetic investigations support magnetization switching through pinning of domain walls.     

Formation of micro- and nanosized particles of the Fe–Al–Co system in water solutions and its magnetic properties

Samples of the Fe–Al–Co system are obtained electrochemically in a water solution. The kinetic dependences that describe the processes that occur in microparticles of aluminum in water solutions are established. The phase composition of the synthesized samples is determined via X-ray diffraction and Mössbauer spectroscopy. It is shown that the main contribution to the fine magnetic structure of Fe–Al–Co is made by the magnetically ordered structure with a hyperfine field around 348 kOe formed by a mechanical mixture of FeCo and Al.