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Paper des Monats
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Characterization of the fcc/bcc orientation relationship by EBSD using pole figures and variants
(2004)
The orientation relationship (OR) between fcc and bcc lattices are described by crystallographic fundamentals using the example of Kurdjumov-Sachs (K-S) and Nishiyama-Wassermann (N-W). Complete pole figures containing all variants will be used to distinguish even between slightly different ORs. EBSD on iron meteorites and duplex steel has been used to analyse a large number of crystal orientations with regard to a high statistical significance and a high probability to capture all variants in a single measurement. It is shown that the use of fixed OR models like K-S, N-W, Bain, Pitsch, or Greninger-Troiano does not satisfacturally reflect the observed experimental pole distributions. It is not convenient to use high-indexed lattice planes and directions to describe the small deviations from the given models. The Euler subspace representation offers a readily comprehensible tool to get an idea about the characteristic of the experimentally detected OR.
Die in zunehmenden Maße Mitte der 80er Jahre einsetzende Substitution von metallischen Materialien z. B. durch hochleistungsfähige polymere Werkstoffe und Verbundwerkstoffe wurde u. a. von der DGM zum Anlass genommen, ihre zukünftigen Aufgaben neu zu definieren und gleichzeitig mit der Gründung des Fachausschusses "Gefüge und Eigenschaften von Polymerwerkstoffen" dieser neuen Entwicklung in der Materialkunde auf dem Gebiet der Kunststoffe und ihrer Anwendungen Rechnung zu tragen.
Structure formation on the surface of indium phosphide irradiated by femtosecond laser pulses
(2005)
Laser-induced periodic surface structures (LIPSS; ripples) with different spatial characteristics have been observed after irradiation of single-crystalline indium phosphide (c-InP) with multiple linearly polarized femtosecond pulses (130 fs, 800 nm) in air. With an increasing number of pulses per spot, N, up to 100, a characteristic evolution of two different types of ripples has been observed, i.e., (i) the growth of a grating perpendicular to the polarization vector consisting of nearly wavelength-sized periodic lines and (ii), in a specific pulse number regime (N = 5-30), the additional formation of equally oriented ripples with a spatial period close to half of the laser wavelength. For pulse numbers higher than 50, the formation of micrometer-spaced grooves has been found, which are oriented perpendicular to the ripples. These topographical surface alterations are discussed in the frame of existing LIPSS theories.
ür die Berücksichtigung mechanischer Belastungen unterhalb der Streckgrenze ist im Rahmen einer zuverlässigen Bauteilauslegung die Kenntnis der elastischen Konstanten von besonderer Bedeutung. Für die experimentelle Bestimmung des Elastizitätsmoduls wurde eine Vielzahl von Verfahren entwickelt, die zum Teil werkstoffspezifisch Eingang in die Normung gefunden haben.
Prinzipiell können diese Verfahren in zwei Gruppen unterteilt werden: die statischen und die dynamischen Prüfverfahren. Die statischen Verfahren beruhen auf der direkten Messung des Spannungs-Dehnungs-Zusammenhangs während einer mechanischen Belastung im elastischen Verformungsbereich (Zug, Biegung, Druck). Die dynamischen Verfahren basieren auf der Schwingungsanregung eines Prüfkörpers und der Analyse der resultierenden Schwingungen (Resonanzmethode oder Impulsanregungsmethode) oder auf der Messung der Ultraschallausbreitungsgeschwindigkeit.
Stellvertretend für die dynamischen Verfahren wird im ersten Teil dieses Beitrages die Resonanzmethode vorgestellt. Der zweite Teil dieses Beitrages fasst die werkstoffabhängigen Ergebnisse der E-Modulbestimmung mit statischen Verfahren im Zug- und Biegeversuch zusammen.
For the safety and cost efficiency of welded high-strength steel structures, precise knowledge of the level and distribution of welding- and cooling-specific stresses and residual stresses is essential, since they exert a decisive influence on strength, crack resistance, and finally on the bearable service load. This paper presents innovative filler materials, of which the phase transformation temperature was deliberately adjusted via the chemical composition. The transformation behaviour of these martensitic Low Transformation Temperature (LTT-) filler materials shows direct effects on the local residual stresses in the weld and the HAZ. These effects can purposefully be exploited to counteract the thermally induced shrinkage of the material and to produce significant compressive residual stresses in the weld. Comparative welding experiments were carried out on 690 MPa high-strength base materials using various LTT-filler materials. High energy synchrotron radiation was used for residual stress measurement. Particularly the use of high energy synchrotron radiation makes it possible to detect the residual stress condition fast without destruction of material. Thereby, residual stress depth gradients can be determined simultaneously without removing material. In steel, gradients of up to 150 µm can be resolved in such a way. Furthermore, the application of high energy radiation permits determination of residual stresses of any available residual austenite contents. Results show significant dependence of transformation temperatures on the resulting residual stress level and distribution.
Cold cracking resistance is a relevant evaluation criterion for welded joints and affected by residual stresses which result from the welding procedure. Compressive residual stresses can thereby have a positive influence on preventing cracking. A unique possibility of generating compressive residual stresses already during the welding procedure is offered by the so-called Low Transformation Temperature (LTT) filler wires. Compared to conventional wires, these materials show decreased phase transformation temperatures which can work against the cooling-specific contraction. In consequence, distinct compressive residual stresses can be observed within the weld and adjacent areas. The strength of these fillers makes them potentially applicable to high-strength steel welding. Investigations were carried out to determine the phase transformation behaviour of different LTT-filler materials. Transformation temperatures were identified using Single Sensor Differential Thermal Analysis (SS-DTA). Additionally Synchrotron radiation was used to measure the transformation kinetics of all involved crystalline phases during heating and cooling of a simulated weld thermal cycle.
Die Analytik von Phthalaten (DMP bis DEHP) in der Luft ist mit thermischer Desorption unter Verwendung von Quarzwolle als Adsorbens erfolgreich realisierbar. Dies wurde durch eine Methodenvalidierung bestätigt. Es wurden sowohl Messungen im Innenraum als auch in Emissionskammern vorgenommen. In den Emissionskammermessungen wurden mögliche Senkeneffekte der Kammeroberfläche (Glas) untersucht. Unter Zuhilfenahme der idealen Abklingkurve wird bestätigt, dass diese Oberfläche eine Senke darstellt.
Phosphorus-based flame retardancy mechanisms - Old hat or a starting point for future development?
(2010)
Different kinds of additive and reactive flame retardants containing phosphorus are increasingly successful as halogen-free alternatives for various polymeric materials and applications. Phosphorus can act in the condensed phase by enhancing charring, yielding intumescence, or through inorganic glass formation; and in the gas phase through flame inhibition. Occurrence and efficiency depend, not only on the flame retardant itself, but also on its interaction with pyrolysing polymeric material and additives. Flame retardancy is sensitive to modification of the flame retardant, the use of synergists/adjuvants, and changes to the polymeric material. A detailed understanding facilitates the launch of tailored and targeted development.
Bisphenol A polycarbonate/acrylonitrile–butadiene–styrene (PC/ABS) with and without bisphenol A bis(diphenyl phosphate) (BDP) and 5 wt.% zinc borate (Znb) were investigated. The pyrolysis was studied by thermogravimetry (TG), TG-FTIR and NMR, the fire behaviour with a cone calorimeter applying different heat fluxes, LOI and UL 94. Fire residues were examined with NMR. BDP affects the decomposition of PC/ABS and acts as a flame retardant in the gas and condensed phases. The addition of Znb results in an additional hydrolysis of PC. The fire behaviour is similar to PC/ABS, aside from a slightly increased LOI and a reduced peak heat release rate, both caused by borates improving the barrier properties of the char. In PC/ABS + BDP + Znb, the addition of Znb yields a borate network and amorphous phosphates. Znb also reacts with BDP to form alpha-zinc phosphate and borophosphates that suppress the original flame retardancy mechanisms of BDP. The inorganic–organic residue formed provides more effective flame retardancy, in particular at low irradiation in the cone calorimeter, and a clear synergy in LOI, whereas for more developed fires BDP + Znb become less effective than BDP in PC/ABS with respect to the total heat evolved.
Structural changes in the condensed phase of bisphenol A polycarbonate (containing 0.45 wt% poly (tetrafluoroethylene))/silicone acrylate rubber/bisphenol A bis(diphenyl-phosphate) (PC/SiR/BDP) and PC/SiR/BDP/zinc borate (PC/SiR/BDP/ZnB) during thermal treatment in nitrogen atmosphere and in fire residues were investigated by solid-state NMR. H-1, B-11, C-13 and P-31 NMR experiments using direct excitation with a single pulse and H-1-P-31 cross-polarization (CP) were carried out including 31P(1 H) and C-13{P-31}double-resonance techniques (REDOR: Rotational Echo Double Resonance) on a series of heat-treated samples (580 K-850 K). Because many amorphous phases occur in the solid residues, and solid-state NMR spectroscopy addresses the most important sites carbon, phosphorus and boron, this paper is the key analytical approach for understanding the pyrolysis and flame retarding phenomenon in the condensed phase of PC/SiR/BDP and PC/SiR/BDP/ZnB.
For the system PC/SiR/BDP it is shown that (i) at temperatures around 750-770 K (main decomposition step) carbonaceous charring of PC occurs and arylphosphate structures are still present, reacted in part with the decomposing PC; (ii) for higher temperatures from 770 K the phosphorus remaining in the solid phase increasingly converts to amorphous phosphonates and inorganic orthophosphates with a minor amount of crystalline orthophosphates; and (iii) H-1-P-31{H-1} CP REDOR and H-1-C-13{P-31} CP REDOR NMR experiments suggest that the phosphates and phosphonates are bound via oxygen to aromatic carbons, indicating the interaction with the carbonaceous char.
When ZnB is added to the system PC/SiR/BDP, (i) ZnB leads to a slightly enhanced PC decomposition for temperatures below 750 K; (ii) alpha-Zn-3(PO4)(2) and borophosphate (BPO4) are formed in small amounts at high temperatures suggesting a reaction between BDP and ZnB during thermal decomposition; and (iii) most of the borate remains in the solid residues, forming an amorphous pure borate network, with the BO3/BO4 ratio increasing with higher temperatures.
The NMR data of thermal and fire residues are highly correlated, underlining the importance of this work for understanding the pyrolysis and flame retardancy mechanisms in the condensed phase during the burning of the PC/SiR blends. (C) 2010 Elsevier Ltd. All rights reserved.