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  • 1
    ISSN: 1436-5073
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary For determination of the crystallographic orientation, of the lattice parameters and of the crystal structure of micro areas of the material surface, a series of radiographic and electronographic techniques are available. Comparison of their effectiveness shows that they are subject to great limitations with regard to their possibilities of application. For this reason, radiographic microdiffraction techniques were developed, of which two were presented. For investigation of selected crystallites in compact samples, the rotatory swivel technique is suitable. In this technique, the intersection lines of the diffraction cones belonging to the network plane systems can be represented with high contrast on a film. The geometry of these diffraction figures was explained and the determination of the crystallographic orientation and of the lattice parameters illustrated by the example of silicone and alpha-iron. For investigation of micro areas of polycrystalline materials, an X-ray microdiffractometer with annular proportional counting tube was used which registers in one go the intensity contained in one Debye-Scherrer ring. With this arrangement, the course of the mechanical tension in front of a cracked tip and the edge of the crack was determined qualitatively.
    Notes: Zusammenfassung Zur Bestimmung der kristallographischen Orientierung, der Gitterparameter und der Kristallstruktur von Mikrobereichen der Werkstoffoberfläche stehen eine Reihe von röntgenographischen und elek-tronographischen Verfahren zur Verfügung. Eine Gegenüberstellung ihrer Leistungsfähigkeit zeigt, daß sie hinsichtlich ihrer Einsatzmöglichkeiten größeren Einschränkungen unterworfen sind. Deshalb wurden neue röntgenographische Mikrobeugungsverfahren entwikkelt, von denen zwei vorgestellt wurden. Zur Untersuchung ausgewählter Kristallite in kompakten Proben ist das Drehschwenkverfahren geeignet, bei dem durch parallele monochromatische Röntgenstrahlung die Schnittlinien der zu den Netzebenenscharen gehörenden Beugungskegel auf einem Film kontrastreich abgebildet werden. Die Geometrie dieser Beugungsfiguren wurde erklärt und die Bestimmung der kristallographischen Orientierung und der Gitterparameter am Beispiel von Si und α-Fe erläutert. Zur Untersuchung von Mikrobereichen polykristalliner Werkstoffe wird ein Röntgenmikrodiffraktometer mit ringförmigem Proportionalzählrohr verwendet, das die in einem Debye-Scherrer-Ring enthaltene Intensität auf einmal registriert. Mit dieser Anordnung wurde der Verlauf der mechanischen Spannung vor einer Rißspitze und an den Rißufern quantitativ ermittelt.
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  • 2
    ISSN: 1436-5073
    Keywords: Key words: TXRF; VPD-ICP-MS; EFTEM; Si wafer; metal contamination.
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract.  The actual detection limits of total reflection X-ray fluorescence (TXRF) are determined and compared to those of destructive physical analytical methods like secondary ion mass spectrometry (SIMS) and chemical methods like vapour phase decomposition in combination with inductively coupled plasma-mass spectrometry (VPD-ICP-MS). The elements Ca, Ti, Cr, Fe, Cu were analyzed on a Si wafer with 10 nm thermal oxide using TXRF and VPD-ICP-MS. The deviation of the TXRF and the VPD-ICP-MS results is less than 30%. The thickness, composition and density of a Co/Ti two-layer stack were determined using angle dependent total reflection and grazing incidence X-ray fluorescence (A-TXRF). The obtained data were compared with X-ray reflectometry (XRR) and energy filtered transmission electron microscopy (EFTEM). The agreement between TEM and A-TXRF is excellent for the determination of the thickness of the metal layers. From these results we conclude, that A-TXRF permits the accurate determination of composition, thickness and density of thin metallic layers. The results are discussed regarding detection efficiency, acquisition time, accuracy and reproducibility.
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  • 3
    ISSN: 1436-5073
    Keywords: EXAFS spectroscopy ; X-ray scattering ; mechanical alloying ; shortrange order
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Amorphous Ni-Ta was obtained by mechanically alloying pure crystalline powders of nickel and tantalum. Structural changes in the local atomic arrangement effected by the mechanical treatment were studied by X-ray scattering and EXAFS spectroscopy. Both X-ray scattering and EXAFS data represent the destruction of long-range order with increasing milling time, i.e., the crystalline-to-amorphous transition. In contrast to an EXAFS study on the Ni-Ti system, our analysis does not confirm the presence of chemical short-range order.
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  • 4
    ISSN: 1436-5073
    Keywords: X-ray divergent beam technique ; pseudo Kossel lines ; computer graphics in X-ray microdiffraction ; determination of lattice constants
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The X-ray interference patterns obtained by the divergent beam transmission technique (pseudo Kossel technique in transmission mode) permit an evaluation of high precision. Especially the low resolution triple intersections appearing in the pattern can be utilized for precise determination of lattice constants. For cubic crystals the parameters can be calculated directly using analytical methods. The computer graphics method is also applicable for crystal systems with low symmetry. It is shown on patterns from LiF obtained with Fe-K and Cu-K radiation that the computer graphics method provides a fast way for the precise determination of lattice constants.
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  • 5
    ISSN: 1436-5073
    Keywords: nitrogen interdiffusion ; austenitic CrNi(Mo) steels ; electron-probe microanalysis (EPMA) ; Kossel technique ; precision determination of lattice parameters
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract For the determination of diffusion coefficients by using the model “diffusion into a plate” methodical examinations were carried out on samples of austenitic steel that had been nitrided in their marginal zones for 1.5 h at 1523 K. For recording of the concentration of N as a function of the distance from the surface electron-probe microanalysis (EPMA) and the precision determination of the lattice parameters by Kossel technique were applied. Both methods yield comparable results.
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  • 6
    Electronic Resource
    Electronic Resource
    Springer
    Microchimica acta 91 (1987), S. 211-218 
    ISSN: 1436-5073
    Keywords: Ti-Mo-N system ; quantitative phase analysis ; EPMA ; XRD
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Arc-melted ternary Ti-Mo-N alloys were heat treated at 1423 K in order to evaluate the compositions of the equilibrium phases. The composition of the bcc phaseβ-Ti x Mo1−x with respect to Mo and Ti was determined by electron probe microanalysis (EPMA) and lattice parameter measurements (XRD). In order to avoid the effects of plastic deformation caused by powdering the ductileβ-Ti x Mo1−x alloys, the lattice parameter measurements were carried out on small particles of the compact samples using Debye-Scherrer cameras. The EPMA and XRD results agree within the expected range of accuracy. Apparently the solubility of nitrogen inβ-Ti x Mo1−x is low and does not perceptibly affect EPMA and XRD results. The relationship between the lattice parameter and the nitrogen content ofδ-TiN1−x was applied to determine the composition ofδ-TiN1−x in equilibrium withβ-TixMo1-x No solid solubility of Mo in TiN1−x could be detected. The tie lines at 1423 K between the two phases were established.
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  • 7
    ISSN: 1436-5073
    Keywords: Kossel pattern ; lattice parameter determination ; diffusion couples ; Ti-N system
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract A Ti/TiN diffusion couple, which had been prepared by isothermal annealing of a Ti sheet in nitrogen atmosphere at 1091 °C and quenched in water, was investigated by Kossel microdiffraction. Kossel patterns were obtained from all phases present in the diffusion couple (α-Ti(N), η-Ti3N2−x, ζ-Ti4N3−x and δ-TiN1-x)It could be shown that the Kossel technique has a superior lateral resolution (10 μm) compared to commercially used X-ray microdiffraction methods, especially in the case of weak X-ray radiation.
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  • 8
    ISSN: 1436-5073
    Keywords: scanning electron microscopy ; X-ray diffraction ; Kossel reflection technique epitaxy
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The characterization of diamonds deposited onto WC single crystals by means of the CVD-method is reported. Investigations were performed by scanning electron microscopy, X-ray diffraction methods and the Kossel reflection technique. Single diamond crystals were deposited in the form of icosahedrons. An orientation correlation between substrate single crystal and diamond crystals could not be proved. In the paper presented, reasons will be given for this fact.
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  • 9
    Electronic Resource
    Electronic Resource
    Springer
    Microchimica acta 68 (1977), S. 167-190 
    ISSN: 1436-5073
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary For binary systems with anteils of the components between 10 and 90%, a very precise concentration determination can be performed via precision measurements of lattice constants. This applies both to intermetallic constants and also to mixed crystals, in some cases even when the atomic radii of the components differ only slightly. The accuracy of the concentration determination can be increased by a closer coupling of the Kossel technique with electron ray microanalysis. In this way, the electron ray methods of microanalytic correction may be checked and improved. The Kossel method is suitable for studying processes in crystallo-graphic phase transformations both in the low temperature and in the high temperature range. Alterations in real structure parameters can be detected, e.g. the density of staggered arrangement. The intensity of Kossel lines, which arise on the A and B sides of AIII BV and AII BVI semiconductors, is distinctly different, so that coupling of Kossel and proton scattering experiments on single crystals may supply new data on crystal physics.
    Notes: Zusammenfassung Für binäre Systeme mit Anteilen der Komponenten zwischen 10 und 90% läßt sich mit der Kossel-Technik über Präzisionsgitter-konstantenmessungen eine sehr genaue Konzentrationsbestimmung durchführen. Das trifft sowohl für intermetallische Verbindungen als auch für Mischkristalle zu; in einigen Fällen gilt das sogar dann, wenn die Atomradien der Komponenten sich nur wenig unterscheiden. Über eine engere Kopplung der Kossel-Technik mit der Elektronenstrahl-Mikroanalyse läßt sich die Genauigkeit der Konzentrationsbestimmung steigern und die elektronenstrahl-mikroanalyti-schen Korrekturverfahren können auf diesem Wege überprüft und verbessert werden. Die Kossel-Technik ist geeignet, die Vorgänge bei kristallogra-phischen Phasenumwandlungen sowohl im Tieftemperaturbereich als auch im Hochtemperaturbereich zu studieren. Sich dabei ändernde Realstrukturparameter, wie z. B. die Versetzungsdichte, lassen sich erfassen. Die Intensität von Kossei-Linien, die an A- und B-Seiten von AIIIBV-bzw. AIIBVI-Halbleitern entstehen, ist deutlich verschieden, so daß sich die Kossel-Technik als ein neues Untersuchungsverfahren für Halbleiteroberflächen anbietet. Die Experimente zur Herstellung von Kossel-Aufnahmen mit Protonenstrahlanregung belegen, daß die Kopplung von Kossei- und Protonenstreuexperimenten an Einkristallen neue kristallphysikalische Aussagen zu liefern vermag.
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  • 10
    ISSN: 1436-5073
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Summary A procedure based on the Kossel technique with which the local dislocation density N at the surface of crystalline substances can be determined in the interval from 107...1010 cm−2 in the microvolume was presented, the width of selected Kossel lines was measured and an assignment of the dislocation densities carried out via calibration samples of the same substance. Besides the requirements of instrument technology, certain geometrical conditions concerning the imaging of the Kossel reflex to be evaluated must be fulfilled. The lateral resolution of the method is at 10μm, and the depth resolution at 2μm. The relative error for the dislocation density is 30%.
    Notes: Zusammenfassung Ein auf der Basis der Kosseitechnik beruhendes Verfahren wurde vorgestellt, mit dem die lokale VersetzungsdichteN im Intervall von 107...1010 cm−2 im Mikrobereich an der Oberfläche von kristallinen Substanzen bestimmt werden kann. Dazu wird die Breite ausgewählter Kossellinien vermessen und eine Zuordnung der Versetzungsdichte über Eichproben der gleichen Substanz vorgenommen. Neben gerätetechnischen Voraussetzungen müssen dabei bestimmte, die Abbildung des auszuwertenden Kosselreflexes betreffende, geometrische Bedingungen erfüllt sein. Das laterale Auflösungsvermögen der Methode liegt bei 10μm Durchmesser, das Tiefenauflösungsvermögen bei 2μm. Der relative Fehler für die Versetzungsdichte beträgt 30%. Mit diesem Verfahren wurden erstmals die Dichte und Verteilung der beim Sintern von Kupfer-Kugel-Platte-Modellen und Kugelschüttungen aus Kupfer in den Sinterkontakten durch Selbstaktivierung entstehenden Versetzungen bestimmt.
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