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Eingeladener Vortrag
- nein (138)
A two-dimensional analysis of the Charpy V-notch specimen subjected to impact loading, according to the standard DIN EN 10045-1, is carried out, using a transient explicit dynamic finite element program. An elastic-viscoplastic, temperature dependent, constitutive relation for a porous plastic solid based on the Gurson damage model is developed. Ductile fracture of the matrix material will be described by the nucleation and subsequent growth of voids to coalescence. An updated Lagrange–Jaumann formulation is employed accounting for large strain and rotation. The discretization is based on four-node plane strain solid elements with one Gauss point. The equations of motion are integrated numerically by an explicit integration algorithm utilising a lumped mass matrix. The predictions of the numerical analysis in terms of force deflection response, crack resistance behaviour and deformation energy absorbtion are compared with results from Charpy tests which were carried out according to the low-blow technique.
In situ FTIR spectroscopy of the Zn-Br battery bromine storage complex at glassy carbon electrodes
(2000)
For the determination of main and minor components in silicon-based ceramic powders, a decomposition by a combustion with elemental fluorine and separation of the volatile fluorination products by a carrier-gas distillation with a subsequent detection by quadrupole mass spectrometry is described. The necessity and success of the separation step is demonstrated for the determination of boron as a minor constituent in SiC, where the spectral interferences of silicon on the boron signals are decreased considerably. The method developed is shown to be directly applicable to determination of silicon in Si3N4, SiC, and SiO2. The determination of nitrogen in Si3N4 requires additional effort, to separate nitrogen from the excess of fluorine. For the determination of boron, a complete mobilization of BF3 is assured by the presence of an adequate amount of GeF4. Analysis results obtained with different types of calibration show a precision of 30 g for boron at the milligram-per-gram level and a precision between 0.5 and 2% (m/m) for the main components, silicon and nitrogen. Within these standard deviations, the results agree well with the values expected from the stoichiometry, with the results for silicon and boron obtained by wet chemical decomposition and slurry techniques in combination with ICP-OES and with the results for nitrogen obtained by carrier gas heat extraction.
Conventional simultaneous thermal analysis, capillary-coupled TGMS, in situ and ex situ Raman and Mössbauer spectroscopy, as well as chemical analysis have been used for the investigation of the first decomposition step of the mixed valence chloroferrate (dmpipzH2)6[Fe(II)Cl4]2[Fe(III)Cl4]2[Fe(II)Cl5][Fe(III)Cl6]. Under argon at ca. 200°C, an almost complete reduction proceeds in a solid state reaction forming Fe(II). It is accompanied by the release of HCl and, to a minor degree, carbon containing species. A multi-phase product with at least two chloroferrate species, coke, and C,H,N-containing polymers is formed. Binuclear iron complexes, such as (dmpipzH)2[Fe(II)2Cl6], and small amounts of (dmpipzH)[Fe(III)Cl4] have been proposed to be the major and minor component of the product mixture, respectively.
PdSn catalysts prepared by various methods and used for nitrate reduction were investigated by means of in situ 119mSn Mössbauer spectroscopy. Characterization by 119mSn Mössbauer spectroscopy revealed significant differences concerning the modification of the palladium particles supported on alumina. The controlled surface reaction preparation method (CSR) leads to formation of PdSn alloys with different tin contents besides small amounts of Sn(II) species and unalloyed metallic Sn. On the other hand the impregnation method leads to a small amount of PdSn alloys and higher contents of Sn(II) species. Sn(IV) species were found in both kinds of catalysts. The CSR prepared PdSn catalysts showed an improved activity and selectivity compared to the catalysts obtained by the impregnation method.
The present study concerns the cleaning of matenats using pulsed laser irradiarton and it summarises the most recent results obtalned by the collaborative research of different European groups, within the kamework of a European program for tralnlng and mobillrv of researchers. A series of pulsed lasers, which emit at various wavelengths (liom UV to IR) wit11 short duration of pulse (few nano-, pico- or fernto-seconds), is used for the removal of metallic, ceramic and organic pollutants kom contaminated solid surfaces of different natures. The scientific results obtained so far are focused on the laser cleaning of silicon wafers from sub-micrometer particles, tile theoretical modelling of particles removal mechanism during dry laser cleaning, the removal of oxide layers from oxidised metals and alloys, as well as on the development of laser imaging as a diagnostrc tool for the estimation of the efficiency of the proposed cleaning technique.
The complexation behaviour of 2,2-bipyridyl-3,3-diol and 2,2-bipyridyl-3-ol, BP(OH)2 and BPOH, with various heavy and transition metal
ions has been investigated in aqueous, alcoholic, and acetonitrile solutions. Whereas the complexes with paramagnetic ions and HgII
are non-fluorescent, ZnII and CdII form highly fluorescent complexes, their coordination geometries depending on the
solvent proticity and hydrogen-bond donating ability. Through a comparative study with the corresponding chelates of 2,2-bipyridyl (bipy),
N,O-coordination in a six-membered ring chelate has been found to be the dominant binding mode in both the ZnII and CdII
complexes in the protic solvents water and ethanol. Only for ZnII and BPOH is exclusive N,N-chelation found in acetonitrile. NMR
measurements on BP(OH)2, BPOH, and bipy in the presence of ZnII and CdII in acetonitrile confirmed these
findings.
The ability and structural requirements of 4-dimethylamino-4-cyano-substituted biphenyls showing photoinduced intramolecular charge transfer (CT) to serve as hydrogen bond- or pH-sensitive fluorescent probes is investigated. The donoracceptor (DA) biphenyls I and II being planar in the CT excited state are most suitable as pH-sensitive fluorescent probes. The two compounds show analytically valuable features such as well-separated absorption and emission bands and signal changes spanning four orders of magnitude and can be employed in ratiometric, self-calibrating, and highly sensitive pH fluorosensing in the range 0<pH<4. Because of an enhanced charge separation in the excited state, the highly twisted DA biphenyl III shows an increased proton sensitivity and can therefore be used to probe solvent proticity ia hydrogen bond formation. The molecular and electronic characteristics of the two types of probes are discussed for the different neutral and acidic alcoholic and/or aqueous solvent mixtures investigated.
Micromachining experiments were performed with Ti:sapphire laser pulses (130 fs - 150 fs, 800 nm, approximately 10 Hz) in air. Employing the direct focusing technique, highly absorbing titanium nitride (TiN) and weakly absorbing polyimide (PI) and polymethylmethacrylate (PMMA) served as target materials. The lateral and vertical precision of the laser ablation and morphological features were characterized by scanning force (SFM), scanning electron (SEM) and optical microscopy. For TiN, incubation can be observed, i.e. the single-pulse surface damage threshold (0.26 J/cm2) is by a factor of two greater than the threshold for 100 pulses. Ablation rates below 10 nm per pulse can be achieved. The evolution of sub-wavelength ripples is presented in dependence on pulse number and laser fluence, respectively. The incubation behavior of the polymers can be described by an accumulation model as for TiN. Experiments on PI with varying focal lengths result in the same modification thresholds. Different polarization states of light (linear, circular) lead to a variation of the ablation rate and to various morphological patterns in the ablation craters (wavelength ripples, cones). Swelling of PMMA occurred at fluences below the ablation threshold.
The influence of hydrogen contained in a sample or otherwise introduced into a glow discharge source (GDS) is here extensively experimentally presented for the case of copper as a sample by means of the addition of small quantities of molecular hydrogen (<1% relative partial pressure) to the argon carrier gas. The progressive addition of molecular hydrogen causes different intensity changes particular to the individual lines of different species such as atomic (Cu I) and ionic (Cu II) copper, and also atomic (Ar I) and ionic (Ar II) argon. Some interesting features of the emission spectrum of hydrogen such as its line, band and even continuum spectrum are observed. It was also found that the depth resolution becomes worse even at very low concentrations of hydrogen.
Im Gegensatz zur Impuls-Echo-Technik, die im Wesentlichen auf der
Anton Erhard, Berlin Reflexion am Fehler basiert, wird bei der Time-Of-Flight Diffraction Technique (TOFD-Technik) die Beugung der Schallwellen am Fehler zum Nachweis genutzt. Zwei Winkelprüfköpfe für Longitudinalwellen sind in V-Durchschallung angeordnet. Die Prüfköpfe befinden sich jeweils auf einer Seite der Schweißnaht und werden bei der Messung parallel zur Schweißnaht verschoben. Das ausgesandte Schallbündel trifft auf Fehlerränder, an denen gebeugte Wellenanteile entstehen, die je nach Entstehungsort mit unterschiedlichen Schalllaufzeiten empfangen, in hochfrequenten A-Bildern abgespeichert und für die Auswertung in B-Bildern dargestellt werden.
Die Untersuchungen zeigen, dass die TOFD-Technik Beiträge zur Fehlergrößenabschätzung liefert, aber keinesfalls die Impuls-Echo-
Technik mit nachgeschalteter Röntgenprüfung ersetzen kann.
Clear evidence of the effects caused by hydrogen, introduced in different forms in an analytical glow discharge source (GDS) operated with argon, is presented for the different matrix elements copper, stainless steel, titanium, aluminium and silicon. When hydrogen is present even in small quantities in argon, not only are there significant changes in the emission line intensities of most elements (analyte and plasma species), but also new spectral features, such as emission bands of new compounds (hydrides of sputtered sample constituents) and a continuous background in the range ~220440 nm. Moreover, the discharge current (the dependent parameter in our experiments) decreases with increasing hydrogen concentration. Different modes of hydrogen introduction, externally in gaseous form or sputtered as a sample constituent, cause very similar effects in terms of discharge current, line intensity (of analyte and plasma gas) and emission continua, which implies similar changes in the discharge processes in the two cases. The excitation of the hydrogen continuum appears to quench the population of the argon metastables (11.55 and 11.72 eV) and, consequently, other elementary processes in the plasma in which the argon metastables take part, but to a different extent for each analyte.
Summary form only given. Machining investigations of crystalline silicon have been performed with laser pulses at a wavelength of 780 nm in the range between 5 fs and 400 fs. Applying 100 pulses per spot, surface damage thresholds were determined by the measurement of the damage diameter. In this pulse duration regime, the threshold fluences were nearly constant. Single-pulse investigations with 5 fs pulses yielded a value of about 0.15 J cm-2 identical to the multi-pulse experiment. This is in contradiction to the behaviour of dielectrics where incubation effects alter the optical properties down to the 5 fs pulse regime. Employing laser pulses with a duration of 130 fs at a wavelength of 800 nm, single-pulse ablation thresholds of 0.23 J cm-2 and 0.16 J cm-2 were determined for Si and InP in air, respectively. The threshold fluence was calculated from the linear relation between the square of the diameters versus the logarithm of the laser fluences.
Aufbereitungsuntersuchungen an schwermetallbelastetem Baggergut aus dem ältesten Kanal Deutschlands
(2000)
Neu entwickelte Gasturbinen werden im Prüffeld mit wechselnden Belastungen beaufschlagt. Dazu wird die Gasturbine mit einer Wasserreibbremse gekoppelt, mit der eine definierte Last erzeugt werden kann.
Ursprünglich war die Wasserreibbremse für eine bestimmte Leistung, die den früheren Leistungen der Gasturbine entsprach, ausgelegt worden. Die erste Prüfung fand im Jahr 1975 statt. Da neuere Gasturbinen wesentlich höhere Leistungen erbringen und die vorhandene Wasserreibbremse weiterhin eingesetzt werden sollte, musste eine Nachqualifizierung vorgenommen werden. Das Ziel war die Absicherung auf eine mögliche Sprödbruchgefahr.
Zunächst wurde eine Studie zur Prüfbarkeit erstellt. An speziellen Testkörpern wurden im Ultraschallabor der BAM Vorversuche zur Machbarkeit, zur Empfindlichkeitsein-stellung und zur Vorbereitung der Prüfung durchgeführt. Dazu wurden spezielle Gruppenstrahlerprüfköpfe gefertigt und ein an die komplizierte Geometrie der Bremsscheiben angepasster Manipulator gebaut. Ferner wurde, um die Prüfzeiten zu reduzieren, die Software zur Datenerfassung und zur Auswertung angepasst.
Im Werk Berlin der Siemens AG wurde in Zusammenarbeit mit der Siemens AG Erlangen eine Ultraschallprüfung mit der Gruppenstahlertechnik der Wasserreibbremse durchgeführt. Überprüft wurde das gesamte Volumen auf axial, radial und tangential beanspruchte Fehler in den Bereichen der Welle und der Bremsscheibe.Die Überprüfung ergab keine relevanten Fehler, so dass die Wasserreibbremse weiterhin eingesetzt werden kann.
Radiation defects in alkaline earth silicate glasses are studied by means of ESR and optical spectroscopies. Previously undiscovered relations between findings of both methods are deduced using four different experimental tools: (i) variation of chemical glass composition; (ii) isochronal annealing of ggr-irradiated samples; (iii) optical bleaching of ggr-irradiated samples; (iv) variation of the ggr-dose. Oxygen hole centres are mainly responsible for the radiation induced absorption in the visible part of the optical spectrum. Previously undescribed electron centres with broad and asymmetric ESR resonances (gprime=1·955) contribute to the optical spectra (2002000 nm) in a small way. It is suggested they are electrons trapped on small aggregates of alkaline earth ions. The radiation induced recharging of incorporated Fe3+ ions is also evidenced by optical and ESR spectroscopies. Fe3+ ions react as electron traps forming not only Fe2+ but also {Fe3+}- species which might be responsible for an absorption band at 300 nm. A correlation was found between the changes of intensity with those of the ESR spectroscopically detected Fe3+ content of the samples.
Entwicklung, Herstellung und Einsatz von Referenzmaterialien für die organische Umweltanalytik
(2000)
Ablation of indium phosphide wafers in air was performed with 130 fs laser pulses at a wavelength of 800 nm at a low repetition rate of 10 Hz. In order to evaluate the role of the incubation effects, the relationship between the number of laser pulses used for the ablation and the threshold fluence was studied. Particular attention was paid to the chemical composition, surface morphology and structural variations of the ablated area.
Bewertung kritischer Befunde bei der Ultraschallprüfung an Schweißnähten mit Modellrechnungen
(2000)
Typische Probleme bei der Schweißnahtprüfung mit Ultrschall entstehen bei ferritischen Werkstoffen vor allem durch Anzeigen von der Nahtkontur, vor allem aus dem Wurzelbereich. Die klassischen Methoden der Unterscheidung formbedingter Anzeigen von Fehlern - z.B. durch Vergleich der A-Bilder von beiden Seten einer Stumpfnaht - können unterstützt werden durch die Modellierung derartiger Anzeigen im Zusammenhang mit hypothetischen Fehlern im wurzelnahen Bereich. Im Beitrag wird die Anwendung vereinfachender Modelle auf diese Problematik vorgestellt und an Beispielen demonstriert.
The movable contact line between two liquids and a gas phase sensitively reacts to small disturbances in the force equilibrium. The shape of the contact line and the adjoining interfaces is determined by the interface and surface tensions, the contact angles, the density differences (hydrostatic pressure), and the Laplace capillary pressure. When these change, the three-phase contact line can deform and even become unstable. Interface and surface tension depend on the concentration and temperature. During mass transport processes (concentration changes) various forms of the instability of the contact line can be observed:
Oscillations of a circular contact line (regular expansion and reduction);
Single deformations (bulges) which quickly disappear again;
Deformations (bulges) which run along the boundary line;
Periodically generated and damped deformations with different modes.
The behavior of the three-phase contact line is of practical importance for coalescence processes and for spontaneous emulsification on liquid surfaces.
Polymere Werkstoffe, insbesondere Faser-Komposite, sind auf der molekularen Skala, aber auch hinsichtlich der Faserorientierung unterschiedlich anisotrop, ebenso ihre mechanischen Eigenschaften. Diese können sich richtungsabhängig um bis zu zwei Größenordnungen unterscheiden, was für die Nutzung der Festigkeit im Leichtbau bedeutend ist. Daher besteht Bedarf an der zerstörungsfreien Charakterisierung der Orientierungs-Parameter der Mikrostruktur: Die neuartige Röntgen-Diffraktions-Rotations-Topographie nutzt (wie alle Röntgen-topographischen Verfahren) einerseits die analytischen Informationen der Röntgenstreuung und erlaubt andererseits die ortsaufgelöste Abbildung dieser Information. Für eine kontinuierliche Erfassung der Orientierungs-Informationen des Probekörpers wird dieser im eng kollimierten monochromatischen Fadenstrahl einer Weitwinkel-Streukammer verfahren. An jeder Position wird das Beugungsbild von einem um den Primärstrahl drehbaren Spalt polar abgetastet, der vor einem großflächigen Röntgen-Detektor positioniert ist. Als Rotations-, Polar- oder Textur-Topogramme werden die Streuintensitäten ortstreu dargestellt. Auswerte-Prozeduren erlauben die Ermittlung von Orientierungs-Verteilungs-Funktionen und statistischen Kennwerten.
Untersuchungs-Beispiele aus einem EU-Projekt zeigen die molekularen Orientierungsverteilungen in thermoplastischen Spritzguß-Komponenten für den Helikopter-Bau, mit Korrelationen zu mechanischen Eigenschaften. Für die ESA wurde die für CFK-Sandwich-Strukturen von Satelliten-Reflektoren erforderliche präzise Orientierung der C-Fasern mit einer Genauigkeit von 0,1 Grad ermittelt. Pro Durchstrahlungsposition werden für die Orientierungs-Information nur wenige Sekunden benötigt. Die verwendete 18 keV Mo-k-a-Strahlung erlaubt Wandstärken bis zu etwa 20 mm.
Die sehr gute Reproduzierbarkeit von tomographischen Messungen zusammen mit den digital vorliegenden Ergebnissen ermöglicht die zerstörungsfreie dreidimensionale quantitative Analyse der untersuchten Bauteile und Proben mit Methoden der Bildverarbeitung. Vorwiegend für den Nachweis von Poren eingesetzt, lassen sich mit CT auch unterschiedliche Materialbestandteile analysieren, wobei die einzige Voraussetzung ein hinreichender Unterschied (es genügen wenige Prozent) in den Röntgenabsorptionseigenschaften der zu unterscheidenden Bestandteile ist.
Mit den in der Bundesanstalt für Materialforschung und -prüfung entwickelten Computertomographieanlagen kann der Anteil von Hohlräumen und Materialbestandteilen einer Probe bestimmt werden, wobei die Größe der nachzuweisenden Bestandteile sich über mehrere Größenordnungen erstreckt.
An ausgewählten Beispielen aus den Bereichen Keramik, Bodenproben und Fahr-bahnübergangssystemen aus Asphalt werden die quantitativen Ergebnisse dargestellt und die in der Bestandteilanalyse erreichbare Genauigkeit diskutiert.
The meaning of calibration in general and in the field of isotopic measurements in particular is described, stressing the fundamental difference between calibration as an aim and tools to achieve calibration. The role of proper uncertainty budgeting as a prerequisite for establishing a calibrated measurement is explained. It leads to the recommendation that the quality of the uncertainty statement should be heavily weighed when ranking or judging calibrated isotopic measurement results evaluated by the Commission on Atomic Weight and Isotopic Abundances.
Two synthetic isotope mixtures for the calibration of sulfur isotope amount ratio measurements were gravimetrically prepared from high purity Ag2S materials enriched in 32S, 33S, and 34S. The mixtures were made so as to closely resemble the (natural) isotopic composition of the materials to be calibrated. This allowed a totally independent evaluation, on the same samples, of the relative combined uncertainty of: (a) the procedure to perform direct measurements of the amount of substance ratios of gas isotopes in the redetermination of the Avogadro constant and (b) the gravimetric preparation procedure. The result of both procedures, mass spectrometry and gravimetry, agree to a relative uncertainty of 3 × 10-4 for sulfur amount ratio measurements of the major abundant isotopes. Thus it seems that a direct measurement of isotopic gas mixtures (e.g. of natural isotopic composition) is now possible for sulfurand probably also for other gaseous isotopeswithout necessarily having to rely on calibration by means of values provided by measurements of gravimetrically prepared isotope mixtures. However, synthetic mixtures may be needed for validation and verification purposes, in particular for quality assurance.
Vergleich HPLC <-> CE
(2000)
Impact
(2000)
Radical species like CO-2,CO-3, SO-2, and SO-3 can be created by exposing natural and synthetic calcium carbonates to sunlight or to the light of a Hg(Xe) lamp. This poses as a risk for ESR dating of these materials, because the radicals formed by light exposure cannot be distinguished from those generated by radioactivity. Furthermore, paramagnetic centers like SO-2, electrons trapped near Zn2+ or Cd2+ ions, surface defects, and radicals with g?=2.0040, can be bleached in ?-irradiated samples by light and show conversion effects.
Three new thiophene derivatives containing different activated ester groups covalently attached to the thiophene ring via a linear undecyl spacer have been synthesized. Electropolymerization of these monomers in acetonitrile led to stable electroactive polymers, while activated functional groups withstand the polymerization conditions and were correctly incorporated in the resulting polymers. These polymers show the characteristic electrochemical behavior of poly(3-alkylthiophene)s with the reversible redox transition in the range of 0.70.9 V. UV/Vis spectra of them exhibit an absorption maximum at around 460 nm. Conductivity measurements on oxidized films of these polymers by means of the two-probe method gave values in the range of 10-310-2 S cm-1. The reactivity of the pendant activated ester groups was demonstrated by the reaction with butylamine, (4-amino-2-oxabutyl) ferrocene and 2-aminoanthraquinone. Spectroscopic studies and electrochemical characterization confirmed that the immobilized amino compounds are covalently bound to the polymer surfaces. These results suggest that the obtained new polymers can be used as electrically conducting carrier materials for the immobilization of biochemically interesting molecules.
Im Rahmen eines Versuchs sollten die Versagensgrenzen eines mit Fluessiggas gefuellten Eisenbahnkesselwagens bei Unterfeuerung ermittelt werden. Untersucht wurden die Auswirkungen eines Unfallfeuers auf einen mit Fluessiggas teilgefuellten Waggon sowie die Konsequenzen, die sich hieraus im Falle eines brandbedingten Berstens hinsichtlich Truemmerflug sowie Druck- und Temperaturbelastung fuer die Umgebung ergeben. Beschrieben werden der Versuchsaufbau, die Versuchsdurchfuehrung sowie wesentliche Ergebnisse und Konsequenzen aus dem Versuch. Unter anderem wird festgehalten, dass durch das Zerbersten des Behaelters mit schlagartiger Verdampfung und anschliessender Zuendung des Fluessiggases Auswirkungen hervorgerufen werden koennen, die im Brandfall in relativ kurzer Zeit eine ernsthafte Gefahr entstehen lassen, und denen durch geeignete sicherheitstechnische Massnahmen begegnet werden sollte.
Gradient Composite Replicas from Protein Crystal Layer Templates produced by Pulsed Laser Deposition
(2000)
Besonders in beweglichen Weichenteilen, wie z.B. Zungen und beweglichen Herzstückspitzen ist die Detektion von Rissen, die zum Bruch des Bauteils führen können, von außerordentlicher Bedeutung. Wegen der komplizierten geometrischen Randbedingungen muß der Schienenprüfzug hier seinen Prüfkopfträger anheben. Aus diesem Grund werden diese Bereiche regelmäßig durch eine manuelle Ultraschallprüfung überwacht. Da auch sehr kleine Anrisse im Oberflächenbereich interessant sind, soll das bereits vorhandene Prüfverfahren durch ein Wirbelstrom-Handprüfsystem so erweitert werden, daß eine sichere Detektion in den gefährdeten Bereichen möglich ist. Aufbau und Wirkungsweise des Wirbelstrom-Handprüfsystems werden erläutert.
Eine berührungslose Abtastung ist bei hoher Prüfgeschwindigkeit unabdingbar. Nur so kann ein Verschleiß der Wirbelstromsonde durch Abrieb verhindert werden.
Gleichzeitig wird eine Beschädigung der zu prüfenden Oberfläche vermieden.
Das Wirbelstromverfahren reagiert empfindlich auf Abstandsänderungen zwischen Wirbelstromsonde und Prüfoberfläche. Eine Trennung des Nutzsignals von dem stö-renden Abstandseffekt gelingt mit Hilfe der Phasenselektion in der Regel nur unzu-reichend. Dieses führt insbesondere bei unebenen Oberflächen zu einer Reduzie-rung der Prüfempfindlichkeit.
Abhilfe schafft eine geregelte Sondenführung, bei der der Abstand konstant gehalten wird.
Es wurden spezielle Sondenhalter nach zwei verschiedenen Verfahren der Ab-standsregelung entwickelt: Ein selbstregelndes System nach dem Luftkissenprinzip sowie ein elektrodynamischer Sondenhalter, angesteuert von einem elektronischen Regler.
Erst durch den Einsatz der geregelten Sondenführung wurde die Detektion kleinster Inhomogenitäten (Ø = 100 µm) innerhalb von Mulden möglich.
Bone development and bone structure depend on surface roughness and structure of metalic implants
(2000)
The physical properties as well as the thickness of the interphase between polymer and reinforcing phase are generally expected to show a strong influence on the macroscopic mechanical properties of composite materials. In this study the scanning force microscope (SFM) has been applied for detecting stiffness gradients near the interface between copper and epoxide. In displacement modulation mode the load exerted by the tip is modulated sinusoidally by vibrating the normal position of the cantilever or the sample. The corresponding amplitude of dynamic cantilever bending is related to local surface stiffness. Thus, using the SFM, the local mechanical properties of the surface under investigation can be probed. When scanning the tip across the reinforcement/polymer interface, the polymeric interphasial zone can be identified with the observed stiffness gradient. For a commercial epoxide based on diglycidyl ether of bisphenol A (DGEBA) cured with an amine-containing hardener, a stiffness gradient was detected that could be fitted by a Gaussian profile typical for diffusional processes. The width of the stiffness gradient was 280 nm. The observation is discussed in terms of interface-induced segregation processes between resin and hardener, as well as heat conduction mechanisms that can occur during the exothermic curing reaction. Both mechanisms are diffusional in nature and, via the local network structure, are expected to show some influence on the local stiffness of the cured epoxy. Copyright © 2000 John Wiley & Sons, Ltd.