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  • 1
    ISSN: 1436-5073
    Keywords: Key words: Auger electron spectroscopy; depth profiling; iron nitride; implantation; plasma.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract.  The depth distribution and the lateral distribution of nitrogen after implantation by means of plasma immersion ion implantation (PIII) in ferritic alloys with 0.3 wt.-% Al and 3.6 wt.-% Cr has been studied by scanning Auger electron spectrometry (AES). To get information about the chemical state of nitrogen and to improve the detection limit methods of data analysis (factor analysis, LLS) have been applied to depth and line profiles, respectively. Thereby the detection limit for nitrogen was reduced from 6% to 1%. The nitrogen distribution is laterally homogeneous in the near surface region only. Depth profiles obtained at several points within the sputter crater showed that the in-depth distribution of nitrogen varies markedly between different points on the sample and from sample to sample. The nitrogen concentration in the implantation maximum corresponds to Fe2N1−x (x ≈ 0.04 ⃛ 0.18). A remarkable feature are grains having a 10 μm wide seam rich in N and a nearly nitrogen-free grain’s interior. The N/Fe ratio determined from line profiles show that the outer layer of the grains has almost the exact composition Fe4N and the transition to the nearly nitrogen-free grain's interior (cN ≤ 1%) occurs within 1 ⃛ 4 μm. The same shape of the N(KLL) peak was found in depth profiles and line scans, respectively, and it corresponds to gasnitrided samples γ ′–Fe4N and ɛ–Fe2N1−x.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Microchimica acta 133 (2000), S. 215-221 
    ISSN: 1436-5073
    Keywords: Key words: PACVD; (Ti ; Al)N hard coatings; oxidation behaviour; laser shock method.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract.  Sputtered (Ti,Al)N hard coatings are successfully used for dry high speed cutting. These films show a lower oxidation rate than TiN or TiC coatings. In our work (Ti,Al)N films were deposited on WC-6%Co substrates at a temperature of 490°C by plasma-assisted chemical vapour deposition (PACVD) using a gas mixture of TiCl4/AlCl3/N2/Ar/H2. Investigation of microstructure, crystalline structure and chemical composition was carried out using SEM, WDXS, TEM, AES and XRD techniques. The chemical composition of the deposited films showed a Al to Ti ratio of 1.33. The film thickness was 5.5 μm. Films showed a fine crystalline size, the metastable fcc crystal structure and a columnar growth. The film surface was under low compressive stress up to several 100 MPa. For (Ti,Al)N/WC-Co compounds the oxidation behaviour up to 1100°C (high temperature range) was studied. Therefore, samples were annealed or rapidly heated in air and under high vacuum condition using the laser shock method. The results show decomposition of the (Ti,Al)N structure to the TiN and the AlN phases at temperature values above 900°C. Heating in air causes growing of a thin aluminum oxide layer at the film surface, which is a barrier for further oxygen diffusion to the alumina-film boundary. Additionally, at temperatures above 900°C oxidation of the WC-6%Co substrate surface was obtained in regions of opened cracks and film delamination.
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  • 3
    ISSN: 1436-5073
    Keywords: MgLi composites ; AES ; factor analysis ; cluster analysis
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract During manufacture of δ-Al2O3 fibre reinforced MgLi alloys the high mobility and reacitivity especially of the Li metal can cause damage of the fibres and loss of the good mechanical behaviour. Because of the low fibre diameter (2 to 5 μm), and the necessity to detect Li, laterally highly resolved Auger electron spectroscopy was used to study the fibre-matrix-interaction. The measurements were performed at sample surfaces, which had been uncovered by in-situ fracture in the UHV apparatus. Due to the bad signal/noise ratio (which was tolerated to achieve high lateral resolution) and the overlapping spectral features, and in order to make an attempt to classify the large amount of spectra obtained, factor analysis in conjuction with cluster analysis was used in the interpretation of AES data. So it was possible to detect the chemical species which are responsible for the apperance of the experimental spectra and to draw conclusions concerning the fracture morphology (inter granular, trans granular).
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Microchimica acta 133 (2000), S. 307-312 
    ISSN: 1436-5073
    Keywords: Key words: Auger electron spectroscopy; data analysis; factor analysis; principal component analysis; depth profiling.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract.  Factor analysis is an established method of peak shape analysis in Auger electron spectrometry. The influence of different commonly used data preprocessing tools onto the results of factor analysis is demonstrated on AES depth profiles of multilayers and implantation profiles. For the analysis of Auger electron spectra it has been traditional to differentiate spectra by Savitzky and Golay’s method to remove background and to elucidate changes in peak shape. For phosphorus implanted in titanium it is shown that background removal works not ideal so that inelastic losses of the Ti(LMM) Auger peak can affect the result of factor analysis for the P(LVV) peak located at ca. 250 eV lower in kinetic energy. The contribution of such losses to the background can be corrected by shifting the spectra so that the high energy side above the peak equals zero. Numerical differentiation can introduce correlated error into the data set. To diminish edge effects the reduction of filter width at the edges and cutting off the outermost data points is recommended. The precision of spectrum reproduction is considered as a crucial test for the number of principal components. The reliability factor is investigated as a measure for the goodness of spectrum reproduction.
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Microchimica acta 133 (2000), S. 17-22 
    ISSN: 1436-5073
    Keywords: Key words: Cu-Ni; thin film; AES; interdiffusion; segregation; oxidation; factor analysis.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract.  The surface and in-depth compositions of sputter-deposited Cu0.57Ni0.42Mn0.01 thin films were studied by Auger electron depth profiling after thermal treatment. The samples were thermally cycled to maximum temperatures of 300 °C to 550 °C in air, argon and forming gas (N2, 5 vol. % H2). Linear least-squares fit to standard spectra and factor analysis were applied to separate the overlapping Auger transitions of Cu and Ni. Under bombardment by 4 keV argon ions, CuNi(Mn) layers display bombardment-induced surface enrichment of Ni in the same extent as binary CuNi alloys. At sufficiently high oxygen partial pressures, a duplex oxide layer is formed and a thick surface copper oxide overgrows the initial nickel oxide. In reducing atmosphere selective oxidation of manganese takes place. A capping NiCr layer prevents CuNi(Mn) from being oxidized, but the film configuration is degraded with increasing annealing temperature due to formation of a surface chromium oxide and diffusion of Ni from the CuNi(Mn) layer into the NiCr/CuNi(Mn) interface.
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  • 6
    ISSN: 1436-5073
    Keywords: Key words: MgLi composites; interfaces; surface analysis; XPS; SIMS; XRD; alumina fibres.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract.  Fibre/matrix interfaces in δ-Al2O3/Mg8Li and δ-Al2O3/Mg composites have been investigated using XPS and SIMS analysis of extracted δ-Al2O3 fibres in context with previous XRD observations. Results obtained indicate that in MgLi based composites lithium enters preferentially the interfacial redox reactions producing Li+ ions that occupy vacant cation positions in the defect δ-Al2O3 lattice which results in a strong fibre/matrix interfacial bond. On the other hand, in Mg matrix composites the magnesium oxide appears to be the final reaction product that does not enter the solid state reaction with adjacent δ-Al2O3 fibre during the melt infiltration process, so that only relatively weak interfacial bond is created.
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  • 7
    ISSN: 1436-5073
    Keywords: AES ; laser ; iron ; nitrogen ; oxygen
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The laser induced modification of iron surfaces with atmospheric species was investigated by means of Auger electron spectroscopy (AES) and scanning electron microscopy (SEM). Different laser systems were used for irradiating iron samples in a wide range of the laser processing parameters up to small foci and ultra short pulses. A nitriding of iron connected with an oxidation of the near surface region was observed in the wavelength range between 193 nm and 10.6 μm using large foci (∼0.1 cm2) and short pulses (10...1400ns). In case of small foci (∼7·10−6cm2) with ns-pulses (50 ns) an enrichment of the iron melt with nitrogen and an advanced oxidation of the surrounding area of the laser spot were detected. When using shorter pulses (200 fs, 40 ps) no indications for a nitriding were found.
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  • 8
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Uncoated and 300 nm pyrocarbon coated polyacrylonitril (PAN) based T300 type carbon fibres were pressure infiltrated with molten Mg8Li and Mg12Li alloys at 903 K and 963 K, respectively, and at contact times of 4 s and 30 s. The fracture surfaces were characterized by in-situ Auger electron spectroscopy (AES) to investigate the reason for differences in mechanical properties, which were obtained by tensile strength experiments. Pressure increase occurred during the fracture of all the MgLi samples under ultra high vacuum conditions in the analyzer chamber of the AES apparatus, indicating porosity probably due to poor wetting of the fibres during the infiltration process. As visible in the scanning electron micrographs, the pyrocarbon coated carbon fibres were less attacked by the molten MgLi than the uncoated fibres. The damage seemed to increase, the higher the Li contents, the higher the contact time and the higher the temperature were chosen, whereas pyrocarbon coating may retard this affection. Characteristic objects of the sample fracture surfaces (fibre fracture surface, fibre jacket surface, fibre impression surface and matrix) were investigated by laterally high resolution Auger electron spectroscopy. Oxygen was found to be distributed all over the fracture surfaces of the as-fractured samples, and Mg/Li were identified in a chemically bound form. On all the characteristic objects carbide (Li2C2) formation has been detected. Factor analysis was performed to exctract the principal components from the whole set of differentiated Auger electron spectra in the Mg/Li, C and O spectral regions, respectively. Cluster analysis of the weighting factors (the factor loadings) of the most important principal components lead to a separation of the data set into two main groups due to the presence or absence of a strong carbide C (KVV) peak as result of Ar+ sputter removal of the covering oxide layer; no separation of the objects concerning the reaction conditions was found.
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