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Autor

  • Günster, Jens (9)
  • Braun, Ulrike (8)
  • Österle, Werner (7)
  • Nolze, Gert (6)
  • Wirth, Cynthia (6)
  • Heinrich, J. (5)
  • Dümichen, Erik (4)
  • Häusler, Ines (4)
  • Rabe, Torsten (4)
  • Wetzel, B. (4)
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  • 2015 (51) (entfernen)

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  • Zeitschriftenartikel (51) (entfernen)

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  • Englisch (51) (entfernen)

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  • EBSD (3)
  • Electron backscatter diffraction (3)
  • LTCC (3)
  • Tribofilm (3)
  • Additive Fertigung (2)
  • Additive manufacturing (2)
  • Automotive exhaust emissions (2)
  • DSC (2)
  • Glass microspheres (2)
  • High temperature corrosion (2)
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Organisationseinheit der BAM

  • 5 Werkstofftechnik (51)
  • 5.1 Materialographie, Fraktographie und Alterung technischer Werkstoffe (16)
  • 5.3 Mechanik der Polymerwerkstoffe (11)
  • 5.4 Keramische Prozesstechnik und Biowerkstoffe (10)
  • 5.2 Experimentelle und modellbasierte Werkstoffmechanik (8)
  • 6 Materialschutz und Oberflächentechnik (7)
  • 5.5 Technische Keramik (5)
  • 5.6 Glas (5)
  • 1 Analytische Chemie; Referenzmaterialien (4)
  • 6.6 Nano-Tribologie und Nanostrukturierung von Oberflächen (4)
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The memory effect in polyolefinic products: A tool for confirming the steam sterilization process (2015)
Bajer, Kamila ; Braun, Ulrike ; Hintersteiner, I.
DSC-Messungen von dampfsterilisierten medizinischen Produkten aus Polyolefinen zeigen beim ersten Heizvorgang als auffällige Besonderheit eine zusätzliche Stufe, bekannt als Temperpeak. Das Ziel dieser Untersuchungen ist, dieses Phänomen nachzuvollziehen und zu verstehen, um es als Nachweis für die Dampfsterilisation nutzen zu können. Dafür wurden PP- und PE-Proben unter verschiedenen Bedingungen dampfsterilisiert und im Ofen thermisch behandelt. Anschließend wurden die Proben mittels DSC untersucht und die Einflüsse der thermischen Behandlung und der mechanischen Beanspruchung analysiert. Um den Einfluss unterschiedlicher Materialspezifikationen zu prüfen, wurden zusätzlich verschiedene Referenzmaterialien (PE und PP) untersucht und GPC-Messungen durchgeführt. Des Weiteren wurde die Beständigkeit des Signals gegenüber der Zeit und der Temperatureinflüssen betrachtet. Die Untersuchungen zeigen, dass sich ein stabiler Memory-Effekt erzeugen lässt.
Water- and boron speciation in hydrous soda-lime-borate glasses (2015)
Bauer, Ute ; Behrens, H. ; Fechtelkord, M. ; Reinsch, Stefan ; Deubener, J.
The structural investigation of hydrated borate glasses provides new insights on the influence of water on boron speciation using spectroscopic methods. In the present study three soda–lime–borate glasses (NCBx with x = 5, 15 and 25 corresponding to xNa2O, 10CaO, 90 - xB2O3 in mol%) were prepared with water content up to 8 wt.%. The water speciation in the glasses was derived by near-infrared (NIR) spectroscopy while boron speciation was investigated by 11B MAS NMR (Magic Angle Spinning Nuclear Magnetic Resonance). For the three glasses effective molar absorption coefficients were determined experimentally for the bands at 5200 cm- 1 and 4600 cm- 1, corresponding to combination modes of H2O molecules and OH-groups, respectively. In contrast to silicate glasses, in which at most ~ 2 wt.% H2O are dissociated to OH-groups, the amount of dissociated H2O may even exceed 5 wt.% in borate glasses. The fraction of tetrahedral to total boron (N4 = BIV / BIV + BIII) is predominantly controlled by the ratio of Na2O + CaO / B2O3, but only weakly affected by the water content of the glasses. When increasing the H2O content from 0 to 8 wt.%, N4 increases from 25% to 26% for NCB5 and from 42% to 47% for NCB25 glasses.
Structuring of LTCC Substrates by a Combination of Pressure-Assisted Sintering and Hot Embossing (2015)
Brandt, Björn ; Rabe, Torsten
A novel technology for the structuring of low temperature co-fired ceramic (LTCC) surfaces is introduced. The commercial LTCC Ceramtape GC is shaped in a zero-shrinkage process by embossing a glass-like carbon mold into the softened LTCC during pressure-assisted sintering. Diverse raised and lowered structures including rings, grids, and characters were fabricated. It was found that de-airing of mold cavities is crucial for the molding of embossments. De-airing is possible through pore channels in the LTCC if embossing is performed at intermediate temperatures. The influence of LTCC viscosity on the mold filling behavior during the formation of raised structures is discussed. For accurate molding and proper densification of the LTCC, hot embossing with 0.41 MPa at 775 °C and subsequent heating under load to 850 °C is proposed. Embossing of precise, 40 µm deep circular cavities and 50 µm high raised bars and characters is demonstrated. Thereby, the high potential of the hot-embossing process for micro-patterning of LTCC is illustrated.
Compilation and evaluation of the pressure-assisted master sintering surface for low-temperature cofired ceramics (2015)
Brandt, Björn ; Rabe, Torsten
Pressure-assisted sintering (PAS) is an established procedure for the production of low-temperature cofired ceramics (LTCC) without lateral shrinkage and minimal shrinkage tolerances for automotive and high-frequency applications. To develop a feasible model for the prediction of densification during that process, master sintering curves (MSCs) for the commercial LTCC DP951 were generated from thermomechanical analysis (TMA) data in the pressure regime from 2 to 500 kPa. Strain mainly related to creep deformation of the LTCC was identified by evaluation of the strain rate and was discarded for the determination of MSC parameters. It was found that no creep occurred at any pressure up to a relative density of 0.9. Different pressure levels can be modeled with the same activation energy of 400 kJ/mol. Densification curves predicted by the model were in good agreement with experimental data. Based on MSCs, the pressure-assisted master sintering surface was compiled to illustrate the influence of pressure on densification. The results show that the MSC approach is a suitable method to feasibly predict the densification of LTCC during PAS.
Sulphurous additives for polystyrene: Influencing decomposition behavior in the condensed phase (2015)
Braun, Ulrike ; Eisentraut, Paul ; Fuchs, S. ; Deglmann, P.
The thermal decomposition behaviour of polystyrene (PS) containing sulphur and phosphorus additives was investigated, using thermogravimetry coupled with Fourier transform infrared spectroscopy (TGA-FTIR). It was found that the additives influence the decomposition process of the polymer in the condensed phase, resulting in a decrease in styrene monomer formation and an increase in styrene oligmer derivatives. Via reference measurements with binary mixtures it was found that the presence of sulphur additives influences the radicalic decomposition process of PS. In combination with quantum chemical calculations it was concluded that this is due to the formation of radicals that abstract hydrogen from the polymer matrix at lower temperatures, disfavouring the radicalic decomposition pathway leading to styrene.
High temperature oxidation behavior of 9-12 % Cr ferritic/martensitic steels in a simulated dry oxyfuel environment (2015)
Chandra, Kamlesh ; Kranzmann, Axel ; Saliwan Neumann, Romeo ; Oder, Gabriele ; Rizzo, F.
The materials in oxyfuel power plant will be subjected to CO2– and SO2–rich gases on the fireside. The oxidation behaviour of two 9–12 % Cr steels T92 and VM12 was studied under dry oxyfuel environment in the temperature range of 580–650 °C for up to 1,000 h. The oxide structure and morphology were analyzed using various experimental techniques. A complex temperature dependence of oxidation rate is observed for both T92 and VM12 whereby the oxidation rate decreased with increasing temperature. This is attributed to increased Cr-enrichment in the inner scale with increasing temperature. T92 and VM12 alloys are also susceptible to carburization in an oxyfuel environment.
Comparative study on high temperature oxidation of T92 steel in dry and wet oxyfuel environments (2015)
Chandra, Kamlesh ; Kranzmann, Axel ; Saliwan Neumann, Romeo ; Rizzo, F.
Fireside oxidation of T92 steel was studied after exposure times up to 1000 h in the temperature range of 580–650 °C in simulated dry (CO2–27 % N2–2 % O2–1 % SO2) and wet (CO2–20 % H2O–7 % N2–2 % O2–1 % SO2) oxyfuel environments. Water vapour addition to the oxyfuel gas substantially increased the oxidation rate. The oxide scales developed under wet environment contained more defects, resulting in higher access of oxidants to the substrate material and enhanced oxidation. In addition, the oxide scales had lower chromium enrichment in the inner layer as compared to that in the dry condition. The oxide scales consisted of hematite and magnetite in the outer layer and a mixture of (Fe, Cr)-spinel, sulphides and wustite in the inner layer. The sulphur distribution differed between the oxide scales developed in dry and wet oxyfuel environments. Sulphur was mainly concentrated in the inner layer and at the oxide/alloy interface. In contrast to the wet oxyfuel gas, very high sulphur concentration was measured in the inner oxide scale formed in the dry oxyfuel gas. Additionally, Fe-sulphide was formed at the interface of inner and outer oxide layer in the wet condition.
Mesoscale modeling of the mechanical and tribological behavior of a polymer matrix composite based on epoxy and 6 vol.% silica nanoparticles (2015)
Dmitriev, A.I. ; Österle, Werner ; Wetzel, B. ; Zhang, G.
A model based on movable cellular automata (MCA) is described and applied for simulating the stress–strain and sliding behavior of a nanocomposite consisting of an epoxy matrix and 6 vol.% of homogeneously distributed silica nanoparticles. Tensile tests were used for verification of the model. It was realized that a slight modification of epoxy properties due to the addition of silica nanoparticles had to be taken into account in order to obtain good correlation between experimental and modeling results. On the other hand, sliding simulations revealed no susceptibility of results to slight modifications of matrix properties, but a significant impact of nanoparticles on the interface structure and smoothness of sliding mechanism. Furthermore, assuming both possibilities, bond breaking and rebinding of automata pairs, can explain different friction levels of polymer materials.
Analysis of polyethylene microplastics in environmental samples, using a thermal decomposition method (2015)
Dümichen, Erik ; Barthel, Anne-Kathrin ; Braun, Ulrike ; Bannick, Claus Gerhard ; Brand, K. ; Jekel, M. ; Senz, R.
Small polymer particles with a diameter of less than 5 mm called microplastics find their way into the environment from polymer debris and industrial production. Therefore a method is needed to identify and quantify microplastics in various environmental samples to generate reliable concentration values. Such concentration values, i.e. quantitative results, are necessary for an assessment of microplastic in environmental media. This was achieved by thermal extraction in thermogravimetric analysis (TGA), connected to a solid-phase adsorber. These adsorbers were subsequently analysed by thermal desorption gas chromatography mass spectrometry (TDS-GC-MS). In comparison to other chromatographic methods, like pyrolyse gas chromatography mass spectrometry (Py-GC-MS), the relatively high sample masses in TGA (about 200 times higher than used in Py-GC-MS) analysed here enable the measurement of complex matrices that are not homogenous on a small scale. Through the characteristic decomposition products known for every kind of polymer it is possible to identify and even to quantify polymer particles in various matrices. Polyethylene (PE), one of the most important representatives for microplastics, was chosen as an example for identification and quantification.
Thermal extraction combined with thermal desorption: A powerful tool to investigate the thermo-oxidative degradation of polyamide 66 materials (2015)
Dümichen, Erik ; Braun, Ulrike ; Kraemer, R. ; Deglmann, P. ; Senz, R.
Using thermogravimetric analysis (TGA) with a solid-phase adsorber for thermal extraction, followed by subsequently analysing the adsorber with thermo-desorption gas chromatography mass spectrometry (TDS-GC–MS) enables measurement of polymer degradation under oxidizing atmosphere, and the identification of certain complex hydrocarbon degradation products by chromatographic separation and defined mass patterns. This technique, thermal-extraction desorption gas chromatography mass spectrometry (TED-GC–MS) was used to investigate the thermo-oxidative degradation of PA 66 and PA 66 doped with 2 wt% of metal oxide particles. In TGA pure PA 66 formed more residue under an oxidizing atmosphere than an inert one. In contrast to the measurements under inert atmosphere, several condensed aromatic species containing nitrogen could be identified in thermo-oxidative measurements. These degradation products were formed through condensation reactions of primary amides originating from imide hydrolysis. The formation of such highly condensed species also causes higher char formation. Four metal oxides have shown an impact on the thermo-oxidative degradation of PA 66: Fe2O3 on η-Al2O3 < pure Fe2O3 = Fe2O3 on γ-Al2O3 < pure ZnO. For ZnO even a char-stabilizing effect could be observed. A catalytic effect of these metal oxides causes more condensed cyclopentanone and pyridine derivates. Thus, more water is formed and released, resulting in increased hydrolysis of the imides and degradation at lower temperatures.
A new molecular understanding of the thermal degradation of PA 66 doped with metal oxides: Experiment and computation (2015)
Dümichen, Erik ; Braun, Ulrike ; Sturm, Heinz ; Kraemer, R. ; Deglmann, P. ; Gaan, S. ; Senz, R.
The thermal molecular degradation of polyamide 66 (PA 66) doped with (partially supported) metal oxide particles (Fe2O3, ZnO, Al2O3) was investigated qualitatively and quantitatively using common analysis techniques like thermogravimetry coupled with IR-spectroscopic evolved gas analysis (TGA-FTIR). Using pyrolysis coupled with gas chromatography mass spectrometry (Py-GC-MS), qualitative conclusions were drawn about the complex hydrocarbon products. However, the combination of TGA with solid-phase extraction, followed by thermal desorption gas chromatography mass spectrometry (TED-GC-MS), allows qualitative and even semi-quantitative conclusions about the decomposition pathway of PA 66 in the presence of various metal oxide particles. The investigations under inert conditions showed that the presence of metal particles increases the rate of decarboxylation and deamination reactions, as well as the formation rate of cyclopentanone and pyridine derivatives. These species are a consequence of various condensation reactions. The condensation reactions release a large amount of water, thus triggering the hydrolysis of PA 66. Molecular thermal degradation mechanisms were developed for the main decomposition as well as for the condensation reactions and supported by quantum chemical calculations. The catalytic effect of the metal oxides in PA 66 increases in the following order: PA 66 = PA 66 – Al2O3 < PA 66 – Fe2O3 < PA 66 – ZnO.
Analyzing the network formation and curing kinetics of epoxy resins by in situ near-infrared measurements with variable heating rates (2015)
Dümichen, Erik ; Javdanitehran, M. ; Erdmann, Maren ; Trappe, Volker ; Sturm, Heinz ; Braun, Ulrike ; Ziegmann, G.
Near-infrared spectroscopy (NIR) turned out to be well suited for analyzing the degree of cure for epoxy systems. In contrast to dynamic scanning calorimetry (DSC), where the released heat of reaction determines the degree of epoxy conversion indirectly, NIR spectroscopy is able to determine the conversion directly by analyzing structural changes. Therefore, a new heatable NIR cell was equipped with an integrated thermocouple, which enables the real sample temperature to be controlled and monitored in situ during epoxy curing. Dynamic scans at different heating rates were used for kinetic modelling, to define kinetic parameters and to predict real curing processes. The kinetic models and their parameters were validated with an isothermal and a more complex multi-step curing scenario. Two available commercial epoxy systems based on DGEBA were used with an anhydride and with an amine hardener. NIR results were compared with DSC data. The simulated conversion predicted with a model fitted on the basis of NIR and DSC dynamic scans showed good agreement with the conversion measured in the isothermal curing validation test. Due to the proven reliability of NIR in measuring the reaction progress of curing, it can be considered a versatile measurement system for in situ monitoring of component production in the automotive, aerospace and wind energy sectors.
Development of bioactive silicate-based glass-ceramics from preceramic polymer and filler (2015)
Elsayed, H. ; Zocca, Andrea ; Bernardo, E. ; Wirth, Cynthia ; Günster, Jens ; Colombo, P.
2014AbstractWollastonite/apatite glass-ceramics have been successfully prepared by a novel approach, consisting of the heat treatment of a silicone resinembedding micro-sized CaCO3particles, that act as reactive fillers, and bioactive glass powder in the SiO2–CaO–P2O5–K2O–Na2O–MgO–CaF2system. Zn-containing silicates, such as hardystonite (Ca2ZnSi2O7) and willemite (Zn2SiO4), were also developed either by directly mixing ZnOpowders with the glass, or by embedding them in the preceramic polymer, as additional fillers.
Sintering and piezoelectric properties of K0.5Na0.5NbO3 glass microspheres (2015)
Hmood, F. J. ; Günster, Jens ; Heinrich, J.
Laser-fused K0.5Na0.5NbO3 (KNN) powder of 75% transparent fraction has been sintered by pressureless sintering, spark plasma sintering (SPS), and hot isostatic pressing (HIP). The laser-fused KNN has a fictive temperature of 503 °C and an onset crystallization temperature of around 529 °C. The results have shown that sintering of the laser-fused KNN powder utilizing the viscous flow of the transparent microspheres (amorphous content)–at the kinetic window (26 °C)–is possible. The highest yield relative density is around 83% at a sintering temperature of 525 °C and at a sintering pressure of 280 MPa. Limited density has been reached because of formation of crystalline surface layers around the amorphous areas. The samples hipped at 525 °C have low piezoelectric coefficient d33 of 5 pC/N because of the residual porosity that led to early dielectric breakdown during the polarization. The sintering behavior, the resulting microstructure as well as the measured properties will be discussed.
Synthesis of porous Si3N4/SiC ceramics with rapid nitridation of silicon (2015)
Hu, H.-L. ; Zeng, Y.-P. ; Zuo, K.-H. ; Xia, Y. ; Yao, Dongxu ; Günster, Jens ; Heinrich, J. ; Li, S.
Porous Si3N4/SiC ceramics were prepared with Si and SiC as raw materials, Y2O3 as sintering additive and ZrO2 as nitrided catalyst through a rapid nitration process. The nitriding rate as a function of temperature and duration was investigated. The porous Si3N4/SiC ceramics with 8 wt% monoclinic ZrO2 addition that was nitrided at 1400 °C for 2 h exhibited the highest nitridation degree of 95%. The experimental results also demonstrated that the reciprocal formation of ZrO2 and ZrN can effectively enhance the level of nitridation by suppressing the melting of silicon in micro-regions. The effects of nitriding time on the mechanical properties of the specimens with ZrO2 as a catalyst was also studied. After nitrided at 1400 °C for various durations from 2 to 8 h, the porous Si3N4/SiC ceramics with the properties of a porosity over 39.8%, a flexural strength over 88.9 MPa and a linear shrinkage lower than 0.6% were achieved. The systematic investigation reveals the catalytic mechanism of ZrO2 in the synthesis of Si3N4/SiC ceramics.
Atomically ordered (Mn,Ga) As crystallites on and within GaAs (2015)
Häusler, Ines ; Moeck, P. ; Volz, K. ; Neumann, W.
Metal organic vapor phase epitaxy (MOVPE) of Mn-rich (Mn,Ga)As on (001) oriented GaAs wafers resulted in atomically ordered (Mn,Ga)As crystallites of two morphological kinds, partially embedded on the wafer surface and fully embedded within the single crystalline matrix. While the former were apparently free of defects (other than unavoidable point defects), the latter contained two domains separated by a grain boundary. Since atomic ordering can be modeled by space group symmetry descent considerations (Bärnighausen trees) that start with the space group of the known crystallographic phases of random (Mn,Ga)As alloys with specified chemical compositions, reasonable structure hypotheses have been derived for two atomically ordered Mn0.75Ga0.25As phases that we call the trigonal α' and the monoclinic β' phases. The implications of these structure hypotheses are in agreement with the results of a range of scanning transmission electron microscopy (STEM) and parallel illumination electron diffraction (ED) studies that include quantitative energy dispersive X-ray spectroscopy, X-ray spectroscopic imaging, as well nanobeam diffraction and high angle precession ED. The coexistence of two domains within the fully embedded crystallites is predicted by the corresponding Bärnighausen tree and observed experimentally for the fully embedded crystallites.
Protecting the structural integrity of composites in fire: Intumescent coatings in the intermediate scale (2015)
Hörold, Andreas ; Schartel, Bernhard ; Trappe, Volker ; Gettwert, V. ; Korzen, Manfred
The fire behaviour of light-weight material used in structural applications is regarded as the main challenge to be solved for mass transportation. The task is to perform realistic experiments, including a mechanical test scenario under fully developed fires, to improve the material's reliability in structural applications. Our approach utilises an intermediate-scale test set-up (specimen size 500 × 500 mm) to apply realistic compressive loads and fully developed fires directly to one side of a carbon-fibre-reinforced sandwich composite. Three different intumescent coatings were applied to sandwich structures and compared to a bench-scale study. The results emphasise intumescent coatings as a promising method to sustain fire resistance, multiplying the time to failure. Nevertheless, the realistic intermediate-scale test using severe direct flame application underlines the extremely short failure times when the actual composite components are tested without any additional insulation.
Constitutive modeling of creep-fatigue interaction for normal strength concrete under compression (2015)
Kindrachuk, Vitaliy ; Thiele, Marc ; Unger, Jörg F.
Conventional approaches to model fatigue failure are based on a characterization of the lifetime as a function of the loading amplitude. The Wöhler diagram in combination with a linear damage accumulation assumption predicts the lifetime for different loading regimes. Using this phenomenological approach, the evolution of damage and inelastic strains and a redistribution of stresses cannot be modeled. The gradual degration of the material is assumed to not alter the stress state. Using the Palmgren–Miner rule for damage accumulation, order effects resulting from the non-linear response are generally neglected. In this work, a constitutive model for concrete using continuum damage mechanics is developed. The model includes rate-dependent effects and realistically reproduces gradual performance degradation of normal strength concrete under compressive static, creep and cyclic loading in a unified framework. The damage evolution is driven by inelastic deformations and captures strain rate effects observed experimentally. Implementation details are discussed. Finally, the model is validated by comparing simulation and experimental data for creep, fatigue and triaxial compression.
Reference measurement procedures for the quatification of platinum-group elements (PGEs) from automotive exhaust emissions (2015)
Labarraque, G. ; Oster, C. ; Fisicaro, P. ; Meyer, Christian ; Vogl, Jochen ; Noordmann, J. ; Rienitz, O. ; Riccobono, F. ; Donet, S.
The major source of the anthropogenic platinum group element (PGE) emission is attributed to the use of catalytic converters in automobiles. This paper describes the work performed by three National Metrology Institutes (Laboratoire national de métrologie et d’essais, by the Physikalisch-technische bundesanstalt, Bundesanatalt für materialforschung und prûfung), in the framework of the Joint Research Project 'PartEmission' under the European Metrology Research Program. An analytical procedure based on a cationic exchange protocol and the isotope dilution or standard addition using an Inductived Coupled Plasma Mass Spectrometer, ICP-MS, for the quantification of the elements Pt, Pd and Rh from automotive exhaust emissions is described. Results obtained on a road dust certified reference (BCR 723) material showed a good agreement with the certified values, at ng/g levels, and relative expanded uncertainties within the range of 7–10%. Analysis of filters impacted with automotive exhaust particle emissions (from a diesel engine) showed the amount of collected PGE at levels of 10–1000 pg/filter. Their quantifications followed the developed analytical protocol that had been carried out with relative expanded uncertainties in the range of a few per cent up to 20% per filter. Nevertheless, a lack of homogeneity between the filters was observed, making the comparison between the project partners difficult in the sake of the validation of their analytical procedures on real samples.
Polyglycerol coated polypropylene surfaces for protein and bacteria resistance (2015)
Lukowiak, M.C. ; Wettmarshausen, Sascha ; Hidde, Gundula ; Landsberger, Petra ; Boenke, Viola ; Rodenacker, K. ; Braun, Ulrike ; Friedrich, Jörg Florian ; Gorbushina, Anna ; Haag, R.
Polyglycerol (PG) coated polypropylene (PP) films were synthesized in a two-step approach that involved plasma bromination and subsequently grafting hyperbranched polyglycerols with very few amino functionalities. The influence of different molecular weights and density of reactive linkers were investigated for the grafted PGs. Longer bromination times and higher amounts of linkers on the surface afforded long-term stability. The protein adsorption and bacteria attachment of the PP-PG films were studied. Their extremely low amine content proved to be beneficial for preventing bacteria attachment.
Slurry-based additive manufacturing of ceramics (2015)
Mühler, T. ; Heinrich, J. ; Wirth, Cynthia ; Günster, Jens
Most additive manufacturing (AM) techniques have in common that material is spread out as thin layers of a dried powder/granulate by a roller or a shaker system. These layers are mostly characterized by a low packing rate. On the other hand, appreciable densities can be reached by the use of ceramic slurries. In this context, the layer-wise slurry deposition (LSD) has been developed. Specific features of the LSD process are reflected on the basis of already existing additive manufacturing technologies. The microstructure of laser-sintered bodies will be discussed, and strategies for an improved microstructure during sintering will be introduced.
Slurry-based powder beds for the selective laser sintering of silicate ceramics (2015)
Mühler, T. ; Wirth, Cynthia ; Ascheri, Mary ; Nicolaides, Dagmar ; Heinrich, J. ; Günster, Jens
Selective laser sintering of ceramic powders is a promising technique for the additive manufacturing of complex- and delicate-shaped ceramic parts. Most techniques have in common that the powder to be sintered is spread to a thin layer as a dry powder by means of a roller or shaker system. These layers have a relatively low density. On the other hand, appreciable densities can be reached with the use of ceramic slurries as the starting material. Therefore, the layer-wise slurry deposition (LSD) process has been developed. Layer stacks, i.e. powder beds, built up by employing the LSD technology exhibit a density comparable to ceramic powder compacts processed by means of conventional forming technologies. Writing the layer information with a focused laser beam in these dense ceramic powder compacts enables the manufacture of ceramic bodies with a high density and precision in contour.
LTCC phase shifters based on tunable ferroelectric composite thick films (2015)
Nikfalazar, M. ; Kohler, C. ; Heunisch, Andreas ; Wiens, A. ; Zheng, Y. ; Schulz, Bärbel ; Mikolajek, M. ; Sohrabi, M. ; Rabe, Torsten ; Binder, R. ; Jakoby, R.
This paper presents, the investigation of tunable components based on LTCC technology, implementing ferroelectric tunable thick-film dielectric. The tunable loaded line phase shifters are fabricated with metal-insulator-metal (MIM) varactors to demonstrate the capabilities of this method for packaging of the tunable components. The MIM varactors consist of one tunable dielectric paste layer that is printed between two silver layers. The tunable ferroelectric paste is optimized for LTCC sintering temperature around 850°C. The phase shifters are fabricated in two different process. They were achieved a figure of merit of 24°/dB (phase shift 192°) at 3 GHz and 18°/dB (phase shift 98°) at 4.4 GHz by using seven unit cells that each unit cell consisting of two MIM varactors.
Microstructural origin of time-dependent changes in alumina sol-gel-coated Inconel 718 exposed to NaCl solution (2015)
Nofz, Marianne ; Zietelmann, Christina ; Feigl, Michael ; Dörfel, Ilona ; Saliwan Neumann, Romeo
Inconel 718 was spin coated twice and fourfold with a sol to obtain 200- and 400-nm-thick transition alumina films on the surface. Bare and sol–gel alumina-coated Inconel 718 samples were exposed to NaCl solution to study their corrosion behavior by means of electrochemical impedance spectroscopy. In combination with scanning electron microscopy, it was shown that bare Inconel 718 is after initial passivation prone to pitting corrosion. For the coated Inconel 718 samples, an improvement in the protective effect of the coatings with time was observed. This observation is in contradiction to the results of other authors who observed degradation of alumina coatings exposed to NaCl solution with time. Transmission electron microscopy revealed a formation of (1) a compacted region at the coating surface as well as (2) a chromium-rich region at the interface between coating and alloy during the contact with a NaCl solution. The last one mainly contributes to the observed chronological sequence of electrochemical characteristics of the samples.
Euler angles and crystal symmetry (2015)
Nolze, Gert
For the description of (single) crystal orientations, e.g. as measured by electron backscatter diffraction (EBSD) & X-ray diffraction (XRD), Euler angles are still generally used to import and export data. However, because of the lack of standard definitions for the unit cell reference settings and specimen axes, several transformation descriptions exist which produce different sets of Euler angles for the same orientation. There is also no recommended region within the minimal Euler orientation space into which orientations should be placed. This is the reason why different sets of Euler angles for the same orientation are generated by the available software packages for indexing EBSD patterns. These issues are reviewed and addressed. The influence of crystal symmetry in form of chiral (enantiomorphic) groups is discussed, as well as how multiple, but symmetry-equivalent sets of Euler angles can be reduced in order to deliver a unique orientation description. The Euler coloring algorithms applied to EBSD map data is critically discussed. The specific case of cubic symmetry, especially the effect of the three-fold rotation on the Euler space is investigated in more detail for the highest-symmetric chiral group 432. Recommendations for standard settings of the unit cell to orthogonal coordinate system transformation are given which exploit inherent symmetry.
Kikuchi pattern analysis of noncentrosymmetric crystals (2015)
Nolze, Gert ; Grosse, C. ; Winkelmann, Aimo
Different models of Kikuchi pattern formation are compared with respect to their applicability to noncentrosymmetric crystals, and the breakdown of Friedel's rule in experimental electron backscatter diffraction (EBSD) patterns is discussed. Different AIIIBV semiconductor materials are used to evaluate the resulting asymmetry of Kikuchi band profiles for polar lattice planes. By comparison with the characteristic etch pit morphology on a single-crystal surface, the polar character of the measured lattice planes can be assigned absolutely. The presented approach enables point-group-resolved orientation mapping, which goes beyond the commonly applied Laue group analysis in EBSD.
Comment on: "Isothermal nature of the B2-B19' martensitic transformation in a Ti-51.2 Ni (at.%) alloy" (2015)
Pelegrina, J.L. ; Yawny, A. ; Olbricht, Jürgen
Fukuda et al. published a paper (Scripta Mater. 68 (2013) 984–987) in which they claimed to be able to determine the isothermal nature of the martensitic transformation in a Ti–Ni alloy. They analyzed the evolution of electrical resistance during isothermal holding stages and concluded that the variations were a consequence of the isothermal transition between austenite and martensite. In the following we will demonstrate that the discussed data do not allow the interpretation presented and that the isothermal nature is not proved.
Transformation activity in ultrafine grained pseudoelastic NiTi wires during small amplitude loading/unloading experiments (2015)
Pelegrina, J.L. ; Yawny, A. ; Olbricht, Jürgen ; Eggeler, G.
Martensitic phase transformations were studied in ultrafine grained Ni-rich pseudoelastic NiTi wires during cyclic deformation under small imposed strain amplitudes. Small strain variation tests were complemented by a thermographic analysis of the emerging temperature distributions in the specimens. The characteristics of the observed thermal profiles result from the specific phase transitions which take place at different stress levels. Homogeneous temperature changes, corresponding to a non-localized transformation activity along the specimen length, were observed throughout the whole range of applied stresses, starting from values as low as 100 MPa. This behavior is in line with previous literature reports for the stress-induced transformation from B2 austenite to R-phase as long as the critical stress for B19' martensite formation is not reached. In the present study, similar type of transformation activity could also be demonstrated at higher strains/stresses, even after the stress induced transformation to B19' was apparently completed. These findings suggest that transformation activity involving the B2 phase is present throughout the whole pseudoelastic stress–strain cycle; i.e., it is not restricted to the initial loading portion. Finally, non-localized transformation to or from B19' was identified during small amplitude strain variations in the plateau-like coexistence ranges of the pseudoelastic cycle.
Nanocrystalline and stacking-disordered beta-cristobalite AlPO4: the now deciphered main constituent of a municipal sewage sludge ash from a full-scale incineration facility (2015)
Peplinski, Burkhard ; Adam, Christian ; Adamczyk, Burkart ; Müller, Ralf ; Michaelis, Matthias ; Krahl, T. ; Emmerling, Franziska
For the first time evidence is provided that a nanocrystalline and stacking-disordered, chemically stabilized β-cristobalite form of AlPO4 occurs in a sewage sludge ash (SSA). This proof is based on a combined X-ray powder diffraction and X-ray fluorescence investigation of an SSA produced at a large-scale fluidized bed incineration facility serving a catching area with a population of 2 million. The structural and chemical characterization was carried out on 'as received' SSA samples as well as on solid residues remaining after leaching this SSA in sodium hydroxide solution. Thus, it was ascertained that the observed nanocrystalline and stacking-disordered cristobalite-like component belongs to the aluminum phosphate component of this SSA, rather than to its silicon dioxide component. In addition, a direct proof is presented that the chemically stabilized β-cristobalite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850°C), typical for fluidized bed incinerators.
A single-crystal co-base superalloy strengthened by gamma' precipitates: structure and mechanical properties (2015)
Petrushin, N. ; Hvatzkiy, K. ; Gerasimov, V. ; Link, T. ; Epishin, A. ; Nolze, Gert ; Gerstein, G.
An experimental Co-base superalloy was designed from the Ni-base system by exchange of Ni and Co concentrations. The alloy consist of a Co-matrix (γ phase) strengthened by cuboidal precipitates Co3(Al,X) (γ' phase). The γ'-solvus temperature is 1?005?°C. [001] single crystals of this alloy were solidified and tested for tension at different temperatures up to 1?000?°C. It was found that the Co-base alloy has a much lower yield stress than a corresponding Ni-base alloy, but a much higher ductility. The partitioning behaviour of the alloying elements in the Co-base alloy and the deformation mechanisms were investigated by scanning and transmission electron microscopy.
Reconstruction of 3D transient temperature field for fusion welding processes on basis of discrete experimental data (2015)
Pittner, Andreas ; Karkhin, Victor ; Rethmeier, Michael
This paper presents an approach to reconstruct the three-dimensional transient temperature field for fusion welding processes as input data for computational weld mechanics. The methodology to solve this inverse heat conduction problem fast and automatically focuses on analytical temperature field models for volumetric heat sources and application of global optimisation. The important issue addressed here is the question which experimental data is needed to guarantee a unique reconstruction of the experimental temperature field. Different computational-experimental test cases are executed to determine the influence of various sets of discrete experimental data on the solvability of the optimisation problem. The application of energy distributions utilised for laser beam welding allows reconstructing the temperature field efficiently. Furthermore, the heat input into the workpiece determined by the simulation contributes to the evaluation of the thermal efficiency of the welding process.
Failure analysis as a tool to optimize the design of a ring on disc tribotest investigating the role of surface roughness (2015)
Pontes Rodrigues, A. C. ; Nunes Ribeiro, P. J. ; Österle, Werner ; de Farias Azevedo, C. R.
The influence of the surface roughness of pearlitic grey cast iron discs on the formation of tribofilms and the evolution of the friction coefficient during a ring on disc tribotest with the addition of magnetite and magnetite–graphite nanopowders as interfacial media was investigated. The roughness parameters of the cast iron discs were varied by electro discharge machining (EDM) and grinding processes, producing four distinct surface roughness conditions. The evolution of the friction coefficient, however, did not reach the steady state for most of the samples and the role of the surface roughness on the friction coefficient could not be identified. Focused ion beam (FIB) microscopy on the cast iron discs was carried out to investigate the microstructure of the discs near the tribosurface. These results showed that the EDM process not only varied the surface roughness, but also changed the microstructure of the cast iron discs, promoting the incipient fusion of the cast iron surface, with the formation of ridges and casting defects (pores). As a result, a layer of rapidly solidified metal with a dendritic microstructure was formed near to the surface of the EDMed discs.
Foreword to topical issue "Low temperature co-fired ceramics -LTCC" (2015)
Rabe, Torsten ; Partsch, U.
Photocleavable epoxy based materials (2015)
Radl, S. ; Kreimer, M. ; Manhart, J. ; Griesser, T. ; Moser, A. ; Pinter, G. ; Kalinka, Gerhard ; Kern, W. ; Schlögl, S.
The present study aims at the development of photodegradable epoxy based materials comprising o-nitrobenzyl ester links that undergo well defined bond cleavage in response to UV irradiation. New bi-functional epoxy based monomers bearing o-nitrobenzyl ester groups are synthesized and thermally cured with an anhydride hardener to yield photosensitive polymers and duromers. The UV induced changes in solubility are exploited for the preparation of positive-type photoresists. Thin patterned films are obtained by photolithographic processes and characterized by microscopic techniques. The results evidence that sensitive resist materials with good resolution and high contrast behavior can be accomplished. Along with resist technology, the applicability of o-nitrobenzyl chemistry in the design of recyclable polymer materials with thicknesses in the millimeter range is evaluated. By monitoring the thermo-mechanical properties upon UV illumination, a distinctive depletion of storage modulus and glass transition temperature is observed with increasing exposure dose. Additionally, single fiber pull-out tests are carried out revealing a significant decrease of the interfacial adhesion at the fiber-matrix interface due to the phototriggered cleavage reaction.
Elastic anisotropy in multifilament Nb3Sn superconducting wires (2015)
Scheuerlein, C. ; Fedelich, Bernard ; Alknes, P. ; Arnau, G. ; Bjoerstad, R. ; Bordini, B.
The elastic anisotropy caused by the texture in the Nb3Sn filaments of PIT and RRP wires has been calculated by averaging the estimates of Voigt and Reuss, using published Nb3Sn single crystal elastic constants and the Nb3Sn grain orientation distribution determined in both wire types by Electron Backscatter Diffraction. At ambient temperature the calculated Nb3Sn E-moduli in axial direction in the PIT and the RRP wire are 130 GPa and 140 GPa, respectively. The calculated E-moduli are compared with tensile test results obtained for the corresponding wires and extracted filament bundles.
Thermally induced crosslinking of poly(N-propargyl glycine) (2015)
Secker, C. ; Brosnan, S.M. ; Limberg, F.R.P. ; Braun, Ulrike ; Trunk, M. ; Strauch, P. ; Schlaad, H.
As polypeptoids become increasingly popular, they present a more soluble and processable alternative to natural and synthetic polypeptides; the breadth of their potential functionality slowly comes into focus. This report analyzes the ability of an alkyne-functionalized polypeptoid, poly(N-propargyl glycine), to crosslink upon heating. The crosslinking process is analyzed by thermal analysis (differential scanning calorimetry and thermogravimetric analysis), Fourier-transform infrared, electron paramagnetic resonance, and solid-state NMR spectroscopy. While a precise mechanism cannot be confidently assigned, it is clear that the reaction proceeds by a radical mechanism that exclusively involves the alkyne functionality, which, upon crosslinking, yields alkene and aromatic products.
Lateral resolution of nanoscaled images delivered by surface-analytical instruments: application of the BAM-L200 certified reference material and related ISO standards (2015)
Senoner, Mathias ; Maaßdorf, A. ; Rooch, Heidemarie ; Österle, Werner ; Malcher, M. ; Schmidt, M. ; Kollmer, F. ; Paul, D. ; Hodoroaba, Vasile-Dan ; Rades, Steffi ; Unger, Wolfgang
The certified reference material BAM-L200, a nanoscale stripe pattern for length calibration and specification of lateral resolution, is described. BAM-L200 is prepared from a cross-sectioned epitaxially grown layer stack of AlxGa1–xAs and InxGa1–xAs on a GaAs substrate. The surface of BAM-L200 provides a flat pattern with stripe widths ranging down to 1 nm. Calibration distances, grating periods and stripe widths have been certified by TEM with traceability to the length unit. The combination of gratings, isolated narrow stripes and sharp edges of wide stripes offers plenty of options for the determination of lateral resolution, sharpness and calibration of length scale at selected settings of imaging surface-analytical instruments. The feasibility of the reference material for an analysis of the lateral resolution is demonstrated in detail by evaluation of ToF-SIMS, AES and EDX images. Other applications developed in the community are summarized, too. BAM-L200 fully supports the implementation of the revised International Standard ISO 18516 (in preparation) which is based on knowledge outlined in the Technical Report ISO/TR 19319:2013.
A new two-stage separation procedure for the IDMS based quantification of low Pd and Pt amounts in automotive exhaust emissions (2015)
Vogl, Jochen ; Meyer, Christian ; Koenig, Maren ; Becker, Dorit ; Noordmann, J. ; Rienitz, O. ; Mamakos, A. ; Riccobono, F.
A two-step separation procedure for the quantification of Pd and Pt in automotive exhaust emissions using isotope dilution mass spectrometry was established using a combination of cation and anion exchange chemistry. AG 50W-X12 was used as cation exchange resin and DGA as weakly basic anion exchange resin. This procedure enabled the effective separation of Pd and Pt from the matrix and from interfering elements. Additionally Pd and Pt were collected in separate chromatographic fractions, which increased the precision of the isotope ratio determination by separate measurements using single collector sector field ICPMS. The analytical procedure was validated by analysing the synthetically prepared samples and the certified reference materials BCR-723 (road dust) and IAEA-450 (algae). For the SI-traceable results complete uncertainty budgets were calculated yielding relatively expanded uncertainties (k = 2) of ≈1% for analyte masses in the ng range. Procedure blanks of 55 pg Pd and 3 pg Pt were obtained. The detection limits were calculated as 12 pg for Pd and 7 pg for Pt. Additionally, Pd and Pt blank levels of different filter materials are presented as well as the first results for automotive exhaust particles collected on cellulose filters.
Element-specific Kikuchi patterns of Rutile (2015)
Vos, M. ; Winkelmann, Aimo ; Nolze, Gert
The kinetic energy of keV electrons backscattered from a rutile (TiO2) surface depends measurably on the mass of the scattering atom. This makes it possible to determine separately the angular distribution of electrons backscattered elastically from either Ti or O. Diffraction effects of these backscattered electrons inside the rutile crystal lead to the formation of Kikuchi patterns. The element-resolved Kikuchi patterns of Ti and O differ characteristically, but each can be described fairly well in terms of the dynamical theory of diffraction. Qualitatively, much of the differences can be understood by considering the relative arrangement of the Ti and O atoms with respect to planes defined by the crystal lattice.
Coating of carbon fibers with adhesion-promoting thin poly(acrylic acid) and poly(hydroxyethylmethacrylate) layers using electrospray ionization (2015)
Wettmarshausen, Sascha ; Friedrich, Jörg Florian ; Meyer-Plath, Asmus ; Kalinka, Gerhard ; Hidde, Gundula ; Weidner, Steffen
Thin coatings of poly(acrylic acid) (PAA) and poly(hydroxyethylmethacrylate) (PHEMA) were deposited onto carbon fibers by means of the electrospray ionization (ESI) technique in ambient air. These high-molecular weight polymer layers were used as adhesion promoters in carbon fiber–epoxy resin composites. Within the ESI process, the carbon fibers were completely enwrapped with polymer in the upper 10 plies of a carbon fiber roving. As identified with scanning electron microscopy also shadowed fibers in a bundle as well as backsides of fiber rovings were pinhole-free coated with polymers (‘electrophoretic effect'). Under the conditions used, the layers have a granular structure. Residual solvent was absent in the deposit. PAA and PHEMA films did not show any changes in composition and structure in comparison with the original polymers as analyzed by X-ray photo-electron spectroscopy and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. Single-fiber pullout tests of coated fibers embedded in epoxy resin showed significantly increased interfacial shear strength. It is assumed that chemical bonds between carbon fiber poly(acrylic acid) and epoxy resin contribute significantly to the improved interactions.
Chirality determination of quartz crystals using electron backscatter diffraction (2015)
Winkelmann, Aimo ; Nolze, Gert
We demonstrate the determination of crystal chirality using electron backscatter diffraction (EBSD) in the scanning electron microscope. The chirality of a-quartz as a space-group-dependent property is verified via direct comparison of experimental diffraction features to simulations using the dynamical theory of electron diffraction.
Point-group sensitive orientation mapping of non-centrosymmetric crystals (2015)
Winkelmann, Aimo ; Nolze, Gert
We demonstrate polarity-sensitive orientation mapping of non-centrosymmetric phases by Electron Backscatter Diffraction (EBSD). The method overcomes the restrictions of kinematic orientation determination by EBSD, which is limited to the centro-symmetric Laue-groups according to Friedel's rule. Using polycrystalline GaP as an example, we apply a quantitative pattern matching approach based on simulations using the dynamical theory of electron diffraction. This procedure results in a distinct assignment of the local orientation according to the non-centrosymmetric point group of the crystal structure under investigation.
Ga+ implantation in a PZT film during focused ion beam micro-machining (2015)
Wollschläger, Nicole ; Österle, Werner ; Häusler, Ines ; Stewart, M.
The objective of the present work was to study the impact of Focused Ion Beam (FIB) machining parameters on the thickness of the damaged layer within a thin film PZT. Therefore, different Ga+- ion doses and ion energies were applied to a standard PZT film (80/20 lead zirconium titanate) under two beam incidence angles (90° and 1°). The thicknesses of the corresponding Ga+-implanted layers were then determined by cross-sectional TEM in combination with energy dispersive spectroscopic (EDS) line-scans and correlated with polarisation hysteresis loops. The results show a decrease of Ga+-implanted layer thickness with decreasing inclination angle, whereas ion energy and ion dose could be correlated with gallium concentration in the implanted layers.. Under the most unfavorable conditions the depth of the affected zone was 26 nm, it was only 2 nm for the most favorable conditions.
Near zero shrinkage porous Al2O3 prepared via 3D-printing and reaction bonding (2015)
Yao, Dongxu ; Wirth, Cynthia ; Zeng, Y.-P. ; Jiang, D. ; Günster, Jens ; Heinrich, J.
Porous Al2O3 with high porosity (~45%), remarkable flexural strength (~70 MPa), and low dimensional change (~1–2%), was produced by indirect 3D printing and reaction bonding. Coarse Al with good flowability was carried out printing green body. The green body was heat treated to get fully oxidized, volume expansion during oxidation simultaneously formed strong neck bonding, not only brought good strength, but also restricted shrinkage. Porous Al2O3 with architecture of macro pores designed by 3D printing and micro pores in the strut formed by packing of particles was obtained. The near zero shrinkage can facilitate precise design of product with complex shape.
Gradient porous silicon nitride prepared via vacuum foaming and freeze drying (2015)
Yao, Dongxu ; Xia, Y. ; Zuo, K.-h. ; Zeng, Y.-P. ; Jiang, D. ; Günster, Jens ; Heinrich, J.G.
Gradient porous silicon nitride (Si3N4) was fabricated by a novel vacuum foaming and freeze drying process. Aqueous Si3N4 slurries were foamed at vacuum pressure of 50–90 kPa, the green body was obtained by the freeze drying process, a gradient pore structure with porosities of 72–90% was achieved after pressureless sintering at 1680 °C. The porosity was increased with decreasing vacuum pressure. The pore structure consists of large pores (~100 μm) on top, medium pores (~45 μm) on the wall of the large pores, and small pores (~0.7 μm) in the matrix. Such gradient porous Si3N4 with macro- and micro-pores has potential application as high temperature filters.
Corrosion of CO2 transport and injection pipeline steels due to the condensation effects caused by SO2 and NO2 impurities (2015)
Yevtushenko, Oleksandra ; Bettge, Dirk ; Bäßler, Ralph ; Bohraus, Stefan
Condensates from the gas stream in simulated CO2 transport pipelines have been identified during the experiments in the laboratory. Because of their acidic origin the corrosion resistance of pipeline steels used for CCS (carbon capture and storage) technology might be limited. Over the last years it has become clear that the amount of water and acid building constituents in the CO2 stream has to be controlled very well. In this work, condensates formed in experiments using gaseous CO2 containing high amounts of water, NO2 and SO2 were analyzed, replicated, and used for extensive electrochemical experiments. These highly acidic condensates were enriched with CO2 and then applied to characteristic steels planned to use in the CCS transport chain. Even high alloy steels are susceptible to localized corrosion under these conditions. The results implicate that condensation of aggressive acid droplets has to be avoided or the locations where condensation takes place have to be controlled extensively.
Formation and function mechanisms of nanostructured tribofilms of epoxy-based hybrid nanocomposites (2015)
Zhang, G. ; Häusler, Ines ; Österle, Werner ; Wetzel, B. ; Jim, B.
The nanostructures and properties of the tribofilms of epoxy (EP) composites filled with short carbon fibers (SCF) and different volume fractions of monodisperse silica nanoparticles were investigated. When the conventional composite filled only with SCF was considered under a high pv condition, an iron oxide layer is formed on the steel counterface. The addition of even only 0.05 vol% nano-silica leads to a significant change of the tribofilm's structure and the tribological behavior of the composite. With increasing silica content, the oxidation layer on the steel surface is gradually replaced by a silica-based tribofilm. A close relationship between the tribofilms’ structure and the tribological behavior of the composites was identified. Mixing, possible reactions and tribo-sintering of silica nanoparticles with other wear products are deemed to be main mechanisms inducing the formation and the lubricity of the silica-based tribofilm.
Impact of counterface topography on the formation mechanisms of nanostructured tribofilm of PEEK hybrid nanocomposites (2015)
Zhang, G. ; Wetzel, B. ; Jim, B. ; Österle, Werner
The effect of steel counterface topography on the formation mechanisms of nanostructured tribofilms of polyetheretherketone (PEEK) hybrid nanocomposites was studied. Three types of surface finishes with mean roughness Ra ranging from nano- to micro-scale were investigated. Tribo-sintering of nanopartides, oxidation of counterface steel and compaction of wear debris are identified to be competing factors dominating the formation and function of the tribofilms. Counterface topography played an important role on the competing factors, and thereby influenced significantly the final structure, the load-carrying capability and the lubrication performance of the tribofilms. It was disclosed that a thin tribofilm, which mainly consists of silica nanoparticles and which forms on the counterface with a submicron roughness, benefits best the tribological performance of the composites
Additive manufacturing of ceramics: Issues, potentialities, and opportunities (2015)
Zocca, Andrea ; Colombo, P. ; Wirth, Cynthia ; Günster, Jens
Additive manufacturing (AM) is a technology which has the potential not only to change the way of conventional industrial manufacturing processes, adding material instead of subtracting, but also to create entirely new production and business strategies. Since about three decades, AM technologies have been used to fabricate prototypes or models mostly from polymeric or metallic materials. Recently, products have been introduced into the market that cannot be produced in another way than additively. Ceramic materials are, however, not easy to process by AM technologies, as their processing requirements (in terms of feedstock and/or sintering) are very challenging. On the other hand, it can be expected that AM technologies, once successful, will have an extraordinary impact on the industrial production of ceramic components and, moreover, will open for ceramics new uses and new markets.
3D-printed silicate porous bioceramics using a non-sacrificial preceramic polymer binder (2015)
Zocca, Andrea ; Elsayed, H. ; Bernardo, E. ; Wirth, Cynthia ; Lopez-Heredia, M.A. ; Knabe, C. ; Colombo, P. ; Günster, Jens
Silicate bioceramics possess an excellent bioactivity; however, shaping them into complex geometries is still challenging. Therefore, this paper aims to present a new strategy for the shaping of a bioglass-ceramic with controlled geometry and properties starting from a glass powder combined with a preceramic polymer, i.e. a silicon resin, and reactive fillers. The powder-based three-dimensional (3D)-printing of wollastonite (CaSiO3)-based silicate bioceramic parts was demonstrated in this work. The resin plays a dual role, as it not only acts as a non-sacrificial binder for the filler powders in the printing process but it also reacts with the fillers to generate the desired bioceramic phases. The mechanical and physical properties, i.e. ball-on-three-balls test, density, porosity and morphology, were evaluated in 3D-printed discs. These samples possessed a total porosity around 64 vol% and a biaxial flexural strength around 6 MPa. The raw materials used in this work also enabled the 3D-printing of scaffolds possessing a designed multi-scale porosity, suitable bioceramic phase assemblage and a compressive strength of 1 MPa (for cylindrical scaffolds with total porosity ~80 vol%). Solubility in TRIS/HCl and in vitro assays, i.e. viability, cytotoxicity and apoptosis assays, were also performed. In vitro tests indicated good cell viability and no cytotoxicity effect on the cells.
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