Thermal study of nickel(II) pyrazolyl complexes

The thermal behavior of the pyrazolyl complexes [NiCl2(HPz) 4] (1), [Ni(NCS)2(HPz)4] (2), [NiCl 2(HdmPz)4]·2H2O (3) and [Ni(NCS) 2(HdmPz)4]·2H2O (4) (HPz=pyrazole, HdmPz=3,5-dimethylpyrazole) has been studied by thermogravimetry (TG) and differential thermal analysis (DTA). The TG data indicated that the thermal stability of [NiX2(HL)4] (X=Cl, NCS) compounds varies depending on the pyrazolyl ligand in the following order HL=HPz>HdmPz. From the thermal decomposition of 3 and 4 it was possible to isolate the intermediate compounds [Ni(μ-Cl)2(HdmPz)2] (3a) and [Ni(μ-1,3-NCS) 2(HdmPz)2] (4a), respectively. The final products of the thermal decompositions of 1-4 were identified as NiO by X-ray powder diffraction. © 2005 Akadémiai Kiadó, Budapest.

Effects of electroplated zinc-nickel alloy coatings on the fatigue strength of AISI 4340 high strength steel

It is well known that fatigue behaviour is an important parameter to be considered in mechanical components subjected to constant and variable amplitude loadings. In combination with corrosion phenomenon, fatigue effects were responsible for proximally 64% of fails that occur in metallic parts of aeronautical accidents in the last 30 years. Recovered substrates have been extensively used in the aerospace field. Cadmium electroplating has been widely applied to promote protective coatings in aeronautical components, resulting in excellent corrosion protection combined with a good performance in cyclic loading. Ecological considerations allied to the increasing demands for corrosion resistance, resulted in the search for possible alternatives. Zinc-nickel alloys received considerable interest recently, since these coatings showed some advantages such as a good resistance to white and red rust, high plating rates and acceptation in the market. In this study the effects of zinc-nickel coatings electroplated on AISI 4340 high strength steel were analysed on rotating bending and axial fatigue strength, corrosion and adhesion resistance. Compressive residual stress field was measured by a X-ray tensometry prior to fatigue tests. Optical microscopy images showed coating thicknesses, adhesion and the existence of an uniform coverage of nearly all substrates. The fractured fatigue specimens were investigated using a scanning electron microscope. Three different zinc-nickel coating thicknesses were tested and comparison with rotating bending fatigue data from specimens cadmium electroplated and heat treated at 190°C for 3, 8 and 24 hours to avoid the diffusion of hydrogen in the substrate, was performed. Experimental results showed effect of coatings on the AISI 4340 steel behaviour when submitted to fatigue testing and the existence of coating thickness influence on the fatigue strength.

Nickel in a tropical soil treated with sewage sludge and cropped with maize in a long-term field study

Sewage sludge produced by the SABESP wastewater treatment plant (Companhia de Saneamento Básico do Estado de São Paulo), located in Barueri, SP, Brazil, may contain high contents of nickel (Ni), increasing the risk of application to agricultural soils. An experiment was carried out under field conditions in Jaboticabal, SP, Brazil, with the objective of evaluating the effects on soil properties and on maize plants of increasing rates of a sewage sludge rich in Ni that had been applied for 6 consecutive years. The experiment was located on a Typic Haplorthox soil, using an experimental design of randomized blocks with four treatments (rates of sewage sludge) and five replications. At the end of the experiment the accumulated amounts of sewage sludge applied were 0.0, 30.0, 60.0 and 67.5 t ha-1. Maize (Zea mays L.) was the test plant. Soil samples were collected 60 d after sowing at depths of 0-20 cm for Ni studies and from 0 to 10 cm and from 10 to 20 cm for urease studies. Sewage sludge did not cause toxicity or micronutrient deficiencies to maize plants and increased grain production. Soil Ni appeared to be associated with the most stable fractions of the soil organic matter and was protected against strong extracting solutions such as concentrated and hot HNO3 and HCl. Ni added to the soil by sewage sludge increased the metal concentration in the shoots, but not in the grain. The Mehlich 3 extractor was not efficient to evaluate Ni phytoavailability to maize plants. Soil urease activity was increased by sewage sludge only in the layer where the residue was applied. © 2006 Elsevier Ltd. All rights reserved.

Slurry sample injection for determination of ferrite nanocolloids chemical composition by ICP spectrometry

This work proposes a new method to determine the chemical composition of magnetic ferrite nanoparticles by the slurry injection technique using the inductively coupled plasma optical emission spectroscopy. In this way, experimental conditions such as aerosol gas flow rate and colloidal stability were optimized in order to use aqueous calibration curves in the slurry nebulization and to determine the chemical composition of a series of sols containing chemically synthesized size-tailored NiFe 2O 4 nanograms. Then, the results of direct sampling and those of conventional aqueous introduction analysis are compared, showing the efficiency of the proposed method.

Magnetoelectric coefficient in strontium ruthenate buffered lanthanum modified bismuth ferrite thin films grown by chemical method

This paper focuses on the magnetoelectric coupling (ME) at room temperature in lanthanum modified bismuth ferrite thin film (BLFO) deposited on SrRuO 3-buffered Pt/TiO 2/SiO 2/Si(100) substrates by the soft chemical method. BLFO film was coherently grown at a temperature of 500 °C. The magnetoelectric coefficient measurement was performed to evidence magnetoelectric coupling behavior. Room temperature magnetic coercive field indicates that the film is magnetically soft. The maximum magnetoelectric coefficient in the longitudinal direction was close to 12 V/cmOe. Dielectric permittivity and dielectric loss demonstrated only slight dispersion with frequency due the less two-dimensional stress in the plane of the film. Polarization reversal was investigated by applying dc voltage through a conductive tip during the area scanning. We observed that various types of domain behavior such as 71 ° and 180° domain switching, and pinned domain formation occurred. Copyright © 2009 American Scientific Publishers All rights reserved.

Retention strength of cobalt-chromium vs nickel-chromium titanium vs Cp titanium in a cast framework association of removable partial overdenture

Aim: There is little information considering the framework association between cast clasps and attachments. The aim of this study was to evaluate the retention strength of frameworks match circumferential clasps and extra resilient attachment cast in three different alloys (cobalt-chromium, nickel-chromium titanium and commercially pure titanium), using two undercut (0.25 and 0.75 mm) and considering different period of time (0, 1/2, 1, 2, 3, 4 and 5 years). Methods: Using two metallic matrices, representing a partially edentulous mandibular right hemiarch with the first molar crown, canine root and without premolars, 60 frameworks were fabricated. Three groups (n = 20) of each metal were cast and each group was divided into two subgroups (n = 10), corresponding the molar undercut of 0.25 mm and 0.75 mm. The nylon male was positioned at the matrix and attached to the acrylic resin of the prosthetic base. The samples were subjected to an insertion and removal test under artificial saliva environment. Results: The data were analyzed and compared with ANOVAs and Tukey's test at 95% of probability. The groups cast in cobaltchromium and nickel-chromium-titanium had the highest mean retention strength (5.58 N and 6.36 N respectively) without significant difference between them, but statistically different from the group cast in commercially pure titanium, which had the lowest mean retention strength in all the periods (3.46 N). The association frameworks using nickel-chromium-titanium and cobalt-chromium could be used with 0.25 mm and 0.75 mm of undercut, but the titanium samples seems to decrease the retention strength, mainly in the 0.75 mm undercut. The circumferential clasps cast in commercially pure titanium used in 0.75 mm undercuts have a potential risk of fractures, especially after the 2nd year of use. Conclusion: This in vitro study showed that the framework association between cast clasp and an extra resilient attachment are suitable to the three metals evaluated, but strongly suggest extra care with commercially pure titanium in undercut of 0.75 mm. Clinical significance: Frameworks fabricated in Cp Ti tend to decrease in retentive strength over time and have a potential risk of fracture in less than 0.75 mm of undercut.

Flexibility and torsional resistance of three nickel-titanium retreatment instrument systems

Aim To assess the dimensional characteristics, flexibility and torsional behaviour of nickel-titanium retreatment instruments. Methodology Using image analysis software and high-resolution digital images, the instrument length, tip angle, diameter at 3mm from the tip and the distance between the blades (pitch length) of the following eight instruments were measured (n=12 for each measurement parameter): the ProTaper Universal retreatment (PTU-R) D1, D2 and D3 instruments; the R-Endo R1, R2 and R3 retreatment instruments; and the Mtwo retreatment (Mtwo-R) sizes 25 and 15 retreatment instruments. Maximum torque and the angular deflection at fracture as well as the bending moment at 45° were measured (n=12) according to the International Standards Organisation (ISO) specification number 3630-1. Data were analysed using the analysis of variance (α=0.05). Results The length of the active part of the instruments was found to vary according to the depth of the canal into which they were designed to reach. The pitch length also increased along the active length. The PTU-R D1 and the Mtwo-R instruments had active tips. Measurements of the bending moment at 45° revealed that the Mtwo-R 15 instrument was the most flexible, whereas the PTU-R D1 was the least flexible. The maximum torque tended to increase as the instrument diameter at 3mm from the tip increased, whereas the angular deflection at fracture varied in the opposite direction. Conclusions The geometrical characteristics of the retreatment instruments and their flexibility and torsion behaviour were consistent with their intended clinical application. © 2011 International Endodontic Journal.

Cu0.5Zn0.5Fe2O4 ferrite for application as a soft magnetic material

This work involved the synthesis and characterization of Cu0.5Zn0.5Fe2O4 ferrite powders prepared by combustion reaction for use as soft magnetic materials. The powders were characterized by nitrogen adsorption (BET), XRD, Rietveld refinement, SEM, TEM and magnetic measures. The results indicate that the combustion reaction yielded crystalline powders containing spinel ferrite as the primary phase and traces of Fe2O3 as secondary phase. The crystallite size and lattice microdeformation calculated from Rietveld refinements were 36 and 0.24 nm, respectively. The micrographic analysis revealed particles smaller than 100 nm and fine particle agglomerates. The particles were approximately spherical and their size, calculated by TEM, was 29 nm. The magnetic parameters indicated that the Cu-Zn ferrite powders presented closed hysteresis loops and soft magnetic properties. © (2012) Trans Tech Publications, Switzerland.

Low-temperature synthesis of nanosized bismuth ferrite by the soft chemical method

This paper describes research on a simple low-temperature synthesis route to prepare bismuth ferrite nanopowders by the polymeric precursor method using bismuth and iron nitrates. BiFeO 3 (BFO) nanopowders were characterized by means of X-ray diffraction analyses, (XRD), Fourier transform infrared (FT-IR) spectroscopy, Raman spectroscopy (Raman), thermogravimnetric analyses (TG-DTA), ultra-violet/vis (UV/Vis) and field emission scanning electron microscopy (FE-SEM). XRD patterns confirmed that a pure perovskite BiFeO 3 structure with a rhombohedral distorted perovskite structure was obtained by heating at 850 °C for 4 hours. Typical FT-IR spectra for BFO powders revealed the formation of a perovskite structure at high temperatures due to a metal-oxygen bond while Raman modes indicated oxygen octahedral tilts induced by structural distortion. A homogeneous size distribution of BFO powders obtained at 850 °C for 4 hours was verified by FE-SEM analyses. © 2012 Elsevier Ltd and Techna Group S.r.l.

Sensor for diuron quantitation based on the P450 biomimetic catalyst nickel(II) 1,4,8,11,15,18,22,25-octabutoxy-29H,31H-phthalocyanine

A biomimetic sensor based on a carbon paste electrode modified with the nickel(II) 1,4,8,11,15,18,22,25-octabutoxy-29H,31H-phthalocyanine complex was developed as a reliable alternative technique for the sensitive and selective analysis of the herbicide diuron in environmental media. The sensor was evaluated using cyclic voltammetry and amperometric techniques. The best amperometric responses were obtained at 750 mV vs. Ag/AgCl (KClsat), using 0.1 mol L-1 phosphate buffer solution at pH 8.0. Under these conditions, the sensor showed a linear response for diuron concentrations between 9.9 × 10-6 and 1.5 × 10-4 mol L -1, a sensitivity of 22817 (±261) μA L mol-1, and detection and quantification limits of 6.14 × 10-6 and 2 × 10-5 mol L-1, respectively. The presence of the nickel complex in the carbon paste improved selectivity, stability, and sensitivity (which increased 700%), compared to unmodified paste. The applicability of the sensor was demonstrated using enriched environmental samples (river water and soil). © 2012 Elsevier B.V. All rights reserved.

Determination of Glycerol in Biodiesel Using a Nickel(II) Oxyhydroxide Chemically Modified Electrode by Cyclic Voltammetry

A glassy carbon electrode chemically modified with nickel oxyhydroxide from a nickel hexacyanoferrate (NiHCF) film was used to determine glycerol in biodiesel by cyclic voltammetry. The modified electrode exhibited a linear response to glycerol concentration in the range from 0.05 to 0.35mmol L-1, and a detection limit of 0.030mmol L-1. The glycerol concentration found in the biodiesel sample was 0.156mmol L-1. The method developed in this study showed a recovery of (100.3±5.0)%. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Tuning the nanostructure of DODAB/nickel tetrasulfonated phthalocyanine bilayers in LbL films

Nanostructured films of dioctadecyldimethylammonium bromide (DODAB) and nickel tetrasulfonated phthalocyanine (NiTsPc) were layer-by-layer (LbL) assembled to achieve a synergistic effect considering the distinct properties of both materials. Prior to LbL growth, the effect of NiTsPc on the structure of DODAB vesicles in aqueous medium was investigated by differential scanning calorimetry (DSC). Therefore, DODAB/NiTsPc LbL films were prepared using NiTsPc at concentrations below and above the limit concentration of vesicle formation according to our DSC experiments. As a result, LbL films with distinct nanostructures were obtained, which were studied at micro and nanoscales by micro-Raman and atomic force microscopy, respectively. A linear growth of the LbL films was observed by ultraviolet-visible absorption spectroscopy. However, the bilayer thickness and the surface morphology of the LbL films were radically affected depending on NiTsPc concentration. The electrostatic interaction between DODAB and NiTsPc was identified via Fourier transform infrared (FTIR) absorption spectroscopy as the main driving force responsible for LbL growth. Because LbL films have been widely applied as transducers in sensing devices, DODAB/NiTsPc LbL films having distinct nanostructures were tested as proof-of-principle in preliminary sensing experiments toward dopamine detection using impedance spectroscopy (e-tongue system). The real capacitance vs. dopamine concentration curves were treated using Principal Component Analysis (PCA) and an equivalent electric circuit, revealing the role played by the LbL film nanostructure and the possibility of building calibration curves. © 2013 Elsevier B.V.

Mechanical properties of vulcanized natural rubber nanocomposites containing functional ceramic nanoparticles

Rubber nanocomposites containing different concentrations of ferroelectric and paramagnetic nanoparticles were fabricated. Nanostructures of ferroelectric potassium strontium niobate and paramagnetic nickel-zinc ferrite were synthesized using a modified polyol method. The nanoparticle characterization was carried out by transmission electron microscopy and X-ray diffraction, showing that the materials were produced with nanometer dimensions, specific crystallinity and microstrain. Mechanical tests such as hardness type Shore A, stress-strain and compression resistance were performed. They showed that increasing the concentration of nanoparticles enhance the rigidity of vulcanized films of natural rubber and this change is more pronounce for the nanocomposites formed with ferrite nanoparticles, likely due to the effect of its morphological and surface properties. © 2013 by American Scientific Publishers.

Influência da adição de nanopartículas paramagnéticas de Ni0,5Zn0,5Fe2O4 nas propriedades estruturais e dielétricas de filmes de borracha natural: preparação e caracterização

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

The fortaleza de minas nickel, copper and platinoids deposit: ore types, tectonics and volcanological aspects

Pós-graduação em Geologia Regional - IGCE