Characterization of laser-nitrided iron and sputtered iron nitride films

Laser-nitriding may be a promising technique for substituting conventional nitriding processes. We have irradiated pure iron with pulses of an excimer laser and achieved high nitrogen contents in a thin surface layer. We found that the nitrogen is dissolved into -Fe, leading to a large amount of retained austenite. This was also verified by X-ray diffraction (XRD) measurements. Three subspectra can be resolved in the Mössbauer spectra (CEMS) for this nitrogen austenite. The nitrogen concentration can be calculated in terms of site occupation, indicating a content as high as 16(1) at%, which is consistent with the results of Rutherford backscattering spectroscopy (RBS), resonant nuclear reaction analysis (RNRA) and Auger electron spectroscopy (AES) measurements. This is more than the solubility limit for -Fe(N). By reactive magnetron-sputtering it is possible to produce thin iron nitride films of various stoichiometries. We report on the production of-Fe _x N and FeN _y films. These films were again characterized by CEMS, RBS, RNRA (¹⁵N(p, )) and XRD. For-Fe _x N, produced in the range 2x3 with medium nitrogen flows during reactive sputtering, the Mössbauer spectra can be well resolved in terms of different iron sites, enabling an accurate calculation of the nitrogen content. For high nitrogen flows during sputtering a phase FeN _y withy>0.5 is produced. This phase is not reported in the Fe-N phase diagram.     

Characterization of magnetic iron oxide nanoparticles

Magnetic nanoparticles have promising applications in many areas, for example optics, electronics, biology, medicine, etc. The main goal of this study is to synthezise and characterize ε-Fe₂O₃ magnetic nanoparticles embedded in amorphous SiO₂ matrix. The Mössbauer spectroscopy analysis of the samples was complemented by the study of X-ray powder diffraction and high-resolution transmission electron microscopy.     

Zinc,chromium and iron silicates as fillers and inorganic colour pigments

Inorganic pigments are characterized by good dispersion and high coating ability. An interesting trend in production of permanent pigment systems may involve a precipitation process followed by roasting of the silica, co-precipitated with metal oxides. The use of zinc silicate may allow elimination of zinc oxide and, partially or even completely, carbon black from rubber mixtures.     

Characterization of iron in airborne particulate matter

In this work soil samples, iron ore and airborne atmospheric particulate matter (PM) in the Metropolitan Region of Belo Horizonte (MRBH), State of Minas Gerais, Brazil, are investigated with the aim of identifying if the sources of the particulate matter are of natural origin, such as, resuspension of particles from soil, or due to anthropogenic origins from mining and processing of iron ore. Samples were characterized by powder X-ray diffraction, X-ray fluorescence and ⁵⁷Fe-Mössbauer spectroscopy. The results showed that soil samples studied are rich in quartz and have low contents of iron mainly iron oxide with low crystallinity. The samples of iron ore and PM have high concentration of iron, predominantly well crystallized hematite. ⁵⁷Fe-Mössbauer spectroscopy confirmed the presence of similar iron oxides in samples of PM and in the samples of iron ore, indicating the anthropogenic origin in the material present in atmosphere of the study area.     

Characterization of chromium‐containing ceramic pigments by XRF and XRD

As no methodology was found in the literature for characterizing ceramic pigments chemically and mineralogically, the present study was undertaken to establish a methodology for the chemical and phase characterization of ceramic pigments by x‐ray fluorescence (XRF) spectrometry and x‐ray diffraction (XRD). In view of the large number of pigments described in the literature (around 44), the present study was limited to characterizing pigments that contained chromium, which is the most versatile chromophore used in ceramics. Copyright © 2004 John Wiley & Sons, Ltd.     

Characterization of reaction products of iron and iron salts and aqueous plant extracts

The complexes formed in aqueous solution as a result of a reaction of iron and iron salts (Fe²⁺ and Fe³⁺) and some plant extracts were analyzed using Mössbauer spectroscopy and Fourier transform infrared. The extracts were obtained from Opuntia elatior mill., Acanthocereus pentagonus (L.) Britton, Mimosa tenuiflora, Caesalpinia coriaria (Jacq.) Willd., Bumbacopsis quinata (Jacq.) Dugand and Acacia mangium Willd., plants growing wildly in different zones of the Isthmus of Panama. Results suggest the formation of mono- and bis-type complexes, and in some cases, the occurrence of a redox reaction. The feasibility of application of the studied extracts as atmospheric corrosion inhibitors is discussed.     

The blue of iron in mineral pigments: a Fe K-edge XANES study of vivianite

Iron is a powerful chromophore element whose pigmenting properties were the first to be recognized among transition metals. The interest in blue iron minerals as pigments for painting was enhanced with the use of vivianite—a natural hydrated ferrous phosphate, Fe₃(PO₄)₂?8H₂O—which in medieval Europe became an alternative to the expensive lapis lazuli, (Na,?Ca)₄(AlSiO₄)₃(SO₄,?Cl,?S), a member of the ultramarines whose appreciated blue tone is due to the presence of sulfur polyanions. Conversely, vivianite coloring is attributed to the intervalence charge transfer (IVCT) Fe²⁺–Fe³⁺ that in later decades was studied by optical techniques and Mössbauer spectroscopy. However, the aging of blue vivianite pigments in old paintings has become a serious concern for conservators, but the aging process still awaits a satisfactory explanation. As an input to this problem, an X-ray absorption near-edge structure (XANES) study at the Fe K-edge of vivianite with different colors and origins was undertaken at the European Synchrotron Radiation Facility using the instrumental facilities of beamline ID-21. The analysis of pre-edge features corroborates previous data on the origin of vivianite color and emphasizes the need for a precautious assessment of iron speciation on the exclusive basis of XANES data. Actual results are discussed and further work is outlined.     

Characterization of iron oxide layers using Auger electron spectroscopy

Metals can form several kinds of oxides. Iron forms wustite (FeO), magnetite (FeO + Fe₂O₃ or Fe₃O₄) and haematite (Fe₂O₃). Iron oxides, especially magnetite, are used for insulation between the lamellas of an electromotor made of electromagnetic sheet. In this work, iron oxide layers were characterized on industrial samples of electromagnetic sheet by AES depth profile analysis, and iron oxides with known chemical composition were used as reference samples, i.e. a magnetite mineral and a standard haematite reference sample. The magnetite mineral was chosen because it can be found in nature in a very pure form. The selection of reference samples was also verified on samples with an oxide layer of known composition, which were prepared by sputter deposition. The composition of the sputtered oxide layers was analysed by the weight-gain method and Rutherford backscattering without the use of standard reference materials (SRM), and the results were then compared with those obtained by AES depth profile analysis.     

Characterization of iron surface modified by 2-mercaptobenzothiazole self-assembled monolayers

A self-assembled monolayer of 2-mercaptobenzothiazole (MBT) adsorbed on the iron surface was prepared. The films were characterized by electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared reflection spectroscopy (FT-IR) and scanning electron microscopy (SEM). Besides, the microcalorimetry method was utilized to study the self-assembled process on iron surface and the adsorption mechanism was discussed from the power-time curve. The results indicated that MBT was able to form a film spontaneously on iron surface and the presence of it could protect iron from corrosion effectively. However, the assembling time and the concentration influence the protection efficiency. Quantum chemical calculations, according to which adsorption mechanism was discussed, could explain the experimental results to some extent.     

Characterization of iron oxy-nitride/nitride double layers on plasma nitrided pure iron by AES depth profiling

A mechanical crater erosion technique is employed to obtain Auger electron spectroscopy (AES) composition-depth profiles of plasma nitrided surface layers on pure iron substrates. The technique is illustrated by the determination of the composition and thickness of the surface layers, and it is shown that after plasma nitriding for 8 h at 570° C in a dissociated NH₃ atmosphere, an iron oxy-nitride layer forms on the surface with a subsequent decrease in thickness of the gamma prime iron-nitride layer below that. The surface roughness of the crater polished in the surface of the material has the largest influence on the accuracy and reproducibility of the depth profiling technique.     

Characterization of pigments used in painting by means of laser-induced plasma and attenuated total reflectance FTIR spectroscopy

The study of pigments which are found in the works of art is one of the most important tasks in the examination of historic, artistic and archaeological materials since it can provide information about their source, the pictorial technique used or the presence of restoration works.In some studies, the historical, artistic and technical characterization of the artefact is not the final goal but its restoration. In those cases, the knowledge about the chemical composition inferred from the analysis of the artwork is crucial for conservators and restorers in order to ensure that the same pigments that were used in the original work are employed for the restoration.In this work, the analytical characterization of a range of different pigments commonly used in art has been carried out using laser-induced plasma (LIBS) and attenuated total reflectance (ATR)-FTIR spectroscopy. The main purpose of this study is to provide a preliminary database of LIBS and ATR-FTIR spectra in order to supply both elemental and molecular information, respectively.     

Characterization of iron oxides and hydroxides in the sand of Flaming Mountain

A sand sample collected at the foot of Flaming Mountain was studied further. On the basis of the change in the relative intensity after heat treatment, one of the sextets observed in its Mössbauer spectrum at liquid nitrogen temperature was ascribed to goethite. This result provides a useful information on the geological history of the region where the mountain is located.     

Characterization of pure and copper-doped iron tartrate crystals grown in silica gel

Single crystal growth of pure and copper-doped iron tartrate crystals bearing composition Cu _x Fe_(1???x)C₄H₄O₆·nH₂O, where x = 0, 0.07, 0.06, 0.05, 0.04, 0.03, is achieved using gel technique. The elemental analysis has been done using energy-dispersive X-ray analysis (EDAX) spectrum. The characterization studies such as Fourier transform infrared spectroscopy (FTIR), powder X-ray diffraction (XRD), magnetic analysis and thermal analysis have been done for crystals with x = 0 for pure iron tartrate and with x = 0.05 for copper-mixed iron tartrate crystals. A detailed comparison has been made between pure and doped crystals.     

Characterization of ultrafine zirconia and iron oxide powders prepared under hydrothermal conditions

Abstract

Nanocrystalline zirconia (6-20 nm) and iron oxide (20-80 nm) powders were produced by hydrothermal treatment of corresponding hydroxides and nitrate solutions. The synthesis parameters (temperature, duration, concentration) allow fabrication of ultrafine oxide powders with various particle size and morphology. The smallest particles were produced by short-time (4-7 s) treatment of nitrate solutions (PH ≈ 1). Prepared nanocrystalline powders exhibit high activity in model solid state reactions.     

Characterization of the end products of the hydrolysis of iron in aqueous solution

A characterization of the iron phases precipitated from aerated solutions of iron(II) sulfate heptahydrate was made using Mössbauer spectroscopy. The experimental conditions for the preparation of the samples were varied. The results are used to the further understanding of rust formation during atmospheric corrosion.     

Characterization of iron counter-ion environment in bulk and supported phosphomolybdic acid based catalysts

Extended X-ray absorption fine structure (EXAFS) was used to characterize the environment of iron counter-cations in Keggin type phosphomolybdic compounds used as catalysts for oxidation reactions. Iron doped compounds corresponding to bulk acid and to acid supported on the cesium salt were prepared and studied. Iron formed hexa-hydrated complex of both Fe³⁺ and Fe²⁺ in the bulk acid, whereas it was present as Fe(OH)₂⁺ hydroxy-cations in the acid supported on the cesium salt. Upon heating the hexa-hydrated complex lost one molecule of water to bind to the Keggin anion through a terminal oxygen. (Fe-O-Mo bond). The environment of the iron hydroxy-cation changed upon heating while its closer coordination append to remained unchanged.     

Raman imaging of human macular pigments

We have imaged the spatial distribution of macular carotenoid pigments (MPs) in the human retina, employing Raman spectroscopy. Using excised human eyecups as initial test samples and resonant excitation of the pigment molecules with narrow-bandwidth blue light from a mercury arc lamp, we record Raman images originating from the carbon-carbon double-bond stretch vibrations of the molecules. Preliminary Raman images reveal significant differences in the MPs of different samples in regard to absolute levels as well as spatial variation. This technique holds promise as a method of rapid screening of MPs in large populations at risk for vision loss from age-related macular degeneration, a leading cause of blindness.     

Computational models for pigments analysis

The main objective of this study is to develop computational models and algorithms for automated image-based characterization of the types of pigments used in watercolours. Pigments constitute the main element of watercolours and such studies can provide important information related to the non-destructive examination of works of art. Semi-transparent pigments are very difficult to discriminate with non-destructive methods due to the reflective properties of the substrate; computer vision techniques can complement such traditional diagnostic methods by computing models and interpreting the visual properties of the pigments used. PACS 07.05.Pj; 42.30.Tz; 42.30.Va; 42.40.My; 89.20.Cf