TY - CONF A1 - Roesch, Philipp A1 - Wittwer, Philipp A1 - Simon, Franz-Georg T1 - CIC & HR-GFMAS: Über Summenparameter in der PFAS-Analytik - Entwicklung von AOF-Parametern anhand Combustion Ion Chromatography N2 - Kurzzsammenfassung der bisherigen Ergebnisse der Vorhaben 4320 und 4390 beim Netzwerktreffen des PerFluSan Netzwerks T2 - Netzwerktreffen PerFluSan CY - Online meeting DA - 19.11.2020 KW - PFAS KW - PFC KW - AOF KW - EOF PY - 2020 AN - OPUS4-51625 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zirnstein, Benjamin A1 - Schulze, Dietmar A1 - Schartel, Bernhard T1 - Combination of phosphorous flame retardants and aluminum trihydrate in multicomponent EPDM composites N2 - Ethylene propylene diene monomer (EPDM) Rubbers with the flame retardants tris(2-ethylhexyl)phosphate, ammonium polyphosphate, polyaniline, and aluminum trihydroxide were prepared and analyzed in this study. The homogenous dispersion of the fillers in the rubber matrix was confirmed by scanning electron microscope. To investigate the interplay of the different flame retardants, the flame retardants were varied systematically. The comprehensive study sought combinations of flame retardants that allow high loadings of flame retardants without deterioration of the physical and mechanical properties of the EPDM rubber. The eight EPDM rubbers were investigated via thermogravimetric analysis and pyrolysis gas chromatography coupled with a mass spectrometer (Py GC/MS) to investigate the potential synergistic effects. In the Py-GC/MS experiments, 27 pyrolysis products were identified. Furthermore, UL 94, limiting oxygen index, FMVSS 302, glow wire tests, and cone calorimeter tests were carried out. In the cone calorimeter test the EPDM rubbers R-1AP and R-1/2P achieved an increase in residue at flameout of 76% and a reduction in total heat evolved of about 35%. Furthermore, the compounds R-1AP and R-1/2P achieved a reduction in MARHE to about 150 kW m−1, a reduction of over 50% compared to the unprotected rubber R. KW - EPDM KW - Rubber KW - Aluminum hydroxide (ATH) KW - Phosphorous flame retardant PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502859 DO - https://doi.org/10.1002/pen.25280 SN - 1548-2634 VL - 60 IS - 2 SP - 267 EP - 280 PB - Wiley AN - OPUS4-50285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cao, L. A1 - Thome, P. A1 - Agudo Jácome, Leonardo A1 - Somsen, C. A1 - Cailletaud, G. A1 - Eggeler, G. T1 - On the influence of crystallography on creep of circular notched single crystal superalloy specimens N2 - The present work contributes to a better understanding of the effect of stress multiaxiality on the creep behavior of single crystal Ni-base superalloys. For this purpose we studied the creep deformation and rupture behavior of double notched miniature creep tensile specimens loaded in three crystallographic directions [100], [110] and [111] (creep conditions: 950 °C and 400 MPa net section stress). Crystal plasticity finite element method (CPFEM) was used to analyze the creep stress and strain distributions during creep. Double notched specimens have the advantage that when one notch fails, the other is still intact and allows to study a material state which is close to rupture. No notch root cracking was observed, while microstructural damage (pores and micro cracks) were frequently observed in the center of the notch root region. This is in agreement with the FEM results (high axial stress and high hydrostatic stress in the center of the notched specimen). Twinning was observed in the notch regions of [110] and [111] specimens, and <112> {111} twins were detected and analyzed using orientation imaging scanning electron microscopy. The present work shows that high lattice rotations can be detected in SXs after creep fracture, but they are associated with the high strains accumulated in the final rupture event. KW - Single crystal Ni-Base superalloys KW - Double notched creep specimen KW - Stress distribution KW - Lattice rotation KW - Cracks PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-506060 DO - https://doi.org/10.1016/j.msea.2020.139255 SN - 0921-5093 VL - 782 SP - 139255 PB - Elsevier B. V. AN - OPUS4-50606 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Szymoniak, Paulina A1 - Kolmangadi, Mohamed Aejaz A1 - Wolf, M. A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Low frequency vibrational density of state of highly permeable super glassy polynorbornenes – The Boson peak N2 - Inelastic incoherent neutron time-of flight scattering was employed to measure the low frequency density of states for a series of addition polynorbornenes with bulky side groups. The rigid main chain in combination with the bulky side groups give rise to a microporosity of these polymers in the solid state. The microporosity characterized by the BET surfaces area varies systematically in the considered series. Such materials have some possible application as active separation layer in gas separation membranes. All investigated materials show excess contributions to the Debye type density of states characteristic for glasses known as Boson peak. The maximum position of the Boson peak shifts to lower frequency values with increasing microporosity. Data for PIM-1 and Matrimid included for comparison are in good agreement to this dependency. This result supports the sound wave interpretation of the Boson peak. KW - Polynorbornes KW - Neutron Scattering PY - 2020 DO - https://doi.org/10.1039/d0cp03360j SN - 1463-9076 VL - 22 IS - 33 SP - 18381 EP - 18387 PB - Royal Chemical Society AN - OPUS4-51165 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina T1 - Spatial Inhomogeneity, Interfaces and Complex Vitrification Behavior of Epoxy and Corresponding Nanocomposites by Broadband Dielectric Spectroscopy and Hyphenated Calorimetry N2 - Polymer nanocomposites (PNCs) with inorganic nanofillers dispersed in a polymer matrix have been widely studied from the 1990s, since the pioneering work by Toyota Central Research. The possibility of producing advanced tailor-made, light weight and low-cost materials, inspired academic and commercial research towards numerous potential applications, facilitating PNCs to become a billion-dollar global industry. The introduction of nanoparticles (NPs) to a polymer matrix is expected to result in improved properties. The outstanding performance of PNCs is determined not only by the characteristics of the used components but also by their phase morphology, including the dispersion of NPs and interfacial properties. Understanding of structure-property relationships is particularly important for polymer nanocomposites with high industrial significance, such as epoxy-based materials reinforced with inorganic nanofillers. These PNCs have been successfully adopted by the marine, automotive and aerospace industries, although they are still rarely studied on a fundamental level. Therefore, this thesis aims for a detailed understanding of the structure, molecular mobility and vitrification kinetics first, of two epoxy-based materials with different network structures and second, of the corresponding nanocomposites with different alumina-based nanofillers. The first system considered (EP/T-LDH) was based on bisphenol A diglycidyl ether (DGEBA) cured with diethylenetriamine (DETA) and taurine-modified layered double hydroxide (T-LDH) NPs. The taurine molecule bears additional functionalities that could enhance the interactions between the matrix and the nanofiller, improving the interphase formation. The seconds system (EP/BNP) was based on DGEBA and methyl tetrahydrophtalic acid anhydride (MTHPA) as a hardener, reinforced with boehmite nanoparticles (BNPs). The comparison of the two systems enables for a comparative study on the effect of different hardeners and the morphology and modification of the alumina-based nanofillers on the material behavior. The materials were investigated employing complementary techniques with different sensitivities and frequency windows. The following methodology was used: transmission electron microscopy (TEM), small – and wide – angle X-ray scattering (SAXS/WAXS), broadband dielectric spectroscopy (BDS), calorimetry in a form of conventional DSC and fast scanning calorimetry (FSC), as well as specific heat spectroscopy (SHS) in a form of temperature modulated DSC, temperature modulated FSC and static FSC by calculating the thermal relaxation rates from the cooperativity approach. The FSC method (based on adiabatic chip calorimetry to probe micrometer-sized samples) was successfully employed in this work, exploiting all its possibilities for the first time in literature for a PNC. Moreover, a systematic analysis technique was established to overcome the problem of vague glass transition regions observed for highly loaded PNCs in the heat flow and heat capacity curves. First, TEM, SAXS/WAXS and indirectly BDS and SHS were employed to obtain the information about the approximate morphology of the PNCs. It was found that epoxy-based materials exhibit a structural heterogeneity in a form of regions with different average crosslinking density. This was indicated by multiple-peak scattering pattern of the polymer matrix and two distinct α-processes (dynamic glass transition) related to the cooperative fluctuation of the epoxy network found by BDS and SHS. This was described for the first time for epoxy-based materials. The two α-relaxations were evidenced differently for the two systems, which is related to different network structures and dipole moments due to the employed hardeners. Nevertheless, structural heterogeneity is an intrinsic feature of these materials, independent of the type of hardener used for the network formation and nanofiller. In addition, matrix inhomogeneities were more pronounced with increasing nanoparticle content. Furthermore, a powerful new technique was applied for X-ray scattering data, using Monte Carlo fits, to describe the NPs dispersion throughout the whole sample volume (as opposed to the local investigations performed by most researches). Additional structural information of the two systems was extracted by BDS and SHS, such as qualitative and quantitative estimation of polymer segments physically adsorbed and/or chemically bonded onto the nanoparticles. Due to the immobilized character of this interphase with respect to the cooperative segmental motions, it is denoted as a rigid amorphous fraction (RAF). For instance, on the contrary to EP/BNP, for EP/T-LDH a dielectrically active process was found, related to the localized fluctuations within RAF. Moreover, the amount of RAF in EP/T-LDH was reaching up to 40 wt % of the system, whereas in EP/BNP it ranged between 1-7 wt %. In the latter case the presence of NPs was found to simultaneously increase and decrease the number of mobile segments, due to the interphase formation and changes in crosslinking density. The difference between the two systems was ascribed to the presence of additional amine functionalities in the T-LDH nanofiller. Second, employing BDS and SHS, a systematic study on the effect of NPs on the segmental dynamics was performed. For example, depending on the nanofiller, the α-processes related to regions with higher crosslinking density was found to shift to higher and lower temperatures with increasing T-LDH and BNPs concentration, respectively. The observed difference is due to the different synergism of the polymer matrix with the nanofiller. Third, a detailed investigation of the vitrification kinetics was performed with DSC and FSC. The concentration dependence of the glass transition temperature was found, similar to the behavior of the α-processes. It was shown that, in parallel to the detected main glass transition, epoxy-based materials can exhibit an additional low temperature vitrification mechanism. As expected from the two distinct α-processes, this behavior was however not discussed in prior studies for an unfilled network former. This finding was correlated to the structural heterogeneity evidenced by other techniques. This thesis, dealing with an in-depth research on the epoxy-based materials that are already successfully employed in numerous applications underlines the necessity of more fundamental research in this field. It shines light on the complexity of these systems and contributes to defining how the structure-property relationships can be determined by combining multiple experimental techniques and analytical methodology. T2 - PhD defense CY - Online meeting DA - 18.12.2020 KW - Interfaces KW - Nanocomposites KW - Rigid amorphous fraction KW - TMDSC KW - BDS PY - 2020 AN - OPUS4-52035 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Omar, Hassan A1 - Qu, Xintong A1 - Schönhals, Andreas T1 - Resolving the mystery of the molecular dynamics of epoxy-based materials using broadband dielectric spectroscopy and hypheneated calorimetry N2 - A detailed calorimetric and dielectric study on two epoxy-based nanocomposite system was performed employing bisphenol A diglycidyl ether (DGEBA) cured with diethylenetriamine (DETA) and methyl tetrahydrophtalic acid anhydride (MTHPA) aas the polymer matrix and taurine-modified MgAL layered double hydroxide (T-LDH) and boehmite as nanofiller. The molecular dynamics investigation revealed an intrinsic structural heterogeneity of the epoxy materials. Moreover the polymer/particle interphase was qualitatively and quantitavely investigated. T2 - Online International Dielectric Society 2020 Workshop CY - Online meeting DA - 28.09.2020 KW - Interfaces KW - Nanocomposites KW - Rigid amorphous fraction KW - BDS KW - TMDSC PY - 2020 AN - OPUS4-51492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adam, Christian A1 - Herzel, Hannes T1 - R-Rhenania - Modifiziertes Rhenania Phosphat aus Klärschlammasche für Bayern N2 - In Bayern wird Klärschlamm aus der kommunalen Abwasserreinigung weitgehend verbrannt. Monoverbrennungsanlagen - ausschließlich für kommunalen Klärschlamm - gibt es in Altenstadt, München, Gendorf, Straubing, Neu-Ulm und zukünftig auch in Augsburg. Die Anlage in Altenstadt verbrennt jährlich ca. 55.000 t Klärschlamm-Trockensubstanz und produziert dabei rund 15.000 t phosphatreiche Aschen. Die Asche aus Altenstadt wird zurzeit überwiegend direkt landwirtschaftlich genutzt. Aufgrund der niedrigen Schadstoffgehalte ist diese Nutzung nach den düngemittelrechtlichen Regelungen gesetzlich zulässig. Um der Intention der neuen Düngeverordnung (26. Mai 2017) nach hocheffizienten, d.h. gut pflanzenverfügbaren Düngemitteln zu entsprechen, ist eine Aufbereitung der Klärschlammasche geplant. Im Rahmen des R-Rhenania Projektes errichten der Betreiber der Klärschlammverbrennungsanlage Altenstadt in Bayern Emter GmbH - und der Düngemittelhersteller sePura GmbH gemeinsam eine AshDec®-Demonstrationsanlage, die im Jahr 2023 den Betrieb aufnehmen soll. Das angewandte AshDec®-Verfahren schließt die Phosphate in der Klärschlammasche thermisch im Drehrohrofen auf und macht diese für Pflanzen vollständig verfügbar. Gleichzeitig werden Schadstoffe wie Arsen, Blei und Cadmium entfernt. Den thermischen Aufschluss kennt man bereits vom erfolgreichen, aber nicht mehr produzierten Düngemittel „Rhenania-Phosphat“, das auf der Basis von Rohphosphaten hergestellt wurde. Die geplante Anlage wird neben den Aschen aus Altenstadt zusätzlich die Aschen aus weiteren bayerischen Verbrennungsanlagen verwerten und für eine Kapazität von 30.000 Jahrestonnen Asche ausgelegt sein. Der Projektpartner sePura plant den produzierten Dünger vollständig in Bayern zu verwerten. Dies verringert die Umweltbelastung durch lange Transportwege und fördert die Regionalität des Vorhabens. T2 - RePhoR Auftaktveranstaltung CY - Online meeting DA - 03.11.2020 KW - Klärschlammasche PY - 2020 AN - OPUS4-51608 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Pauw, Brian Richard A1 - Szymoniak, Paulina T1 - Dataset and Jupyter worksheet interpreting the (results from) small- and wide-angle scattering data from a series of boehmite/epoxy nanocomposites. Accompanies the publication "Competition of nanoparticle-induced mobilization and immobilization effects on segmental dynamics of an epoxy-based nanocomposite" N2 - Dataset and Jupyter worksheet interpreting the (results from) small- and wide-angle scattering data from a series of boehmite/epoxy nanocomposites. Accompanies the publication "Competition of nanoparticle-induced mobilization and immobilization effects on segmental dynamics of an epoxy-based nanocomposite", by Paulina Szymoniak, Brian R. Pauw, Xintong Qu, and Andreas Schönhals. Datasets are in three-column ascii (processed and azimuthally averaged data) from a Xenocs NanoInXider SW instrument. Monte-Carlo analyses were performed using McSAS 1.3.1, other analyses are in the Python 3.7 worksheet. Graphics and result tables are output by the worksheet. KW - Small angle scattering KW - X-ray scattering KW - Nanocomposite KW - Polymer nanocomposite KW - Boehmite KW - Analysis KW - SAXS/WAXS PY - 2020 DO - https://doi.org/10.5281/zenodo.4321087 PB - Zenodo CY - Geneva AN - OPUS4-51829 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Schönauer-Kamin, D. A1 - Moos, R. A1 - Reimann, T. A1 - Giovannelli, F. A1 - Rabe, Torsten T1 - Influence of pressure and dwell time on pressure‐assisted sintering of calcium cobaltite N2 - Calcium cobaltite Ca3Co4O9, abbreviated Co349, is a promising thermoelectric material for high‐temperature applications in air. Its anisotropic properties can be assigned to polycrystalline parts by texturing. Tape casting and pressure‐assisted sintering (PAS) are a possible future way for a cost‐effective mass‐production of thermoelectric generators. This study examines the influence of pressure and dwell time during PAS at 900°C of tape‐cast Co349 on texture and thermoelectric properties. Tape casting aligns lentoid Co349. PAS results in a textured Co349 microstructure with the thermoelectrically favorable ab‐direction perpendicular to the pressing direction. By pressure variation during sintering, the microstructure of Co349 can be tailored either toward a maximum figure of merit as required for energy harvesting or toward a maximum power factor as required for energy harvesting. Moderate pressure of 2.5 MPa results in 25% porosity and a textured microstructure with a figure of merit of 0.13 at 700°C, two times higher than the dry‐pressed, pressureless‐sintered reference. A pressure of 7.5 MPa leads to 94% density and a high power factor of 326 µW/mK2 at 800°C, which is 11 times higher than the dry‐pressed reference (30 MPa) from the same powder. KW - Hot pressing KW - Texture KW - Thermoelectric properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515973 DO - https://doi.org/https://doi.org/10.1111/jace.17541 SN - 0002-7820 VL - 104 IS - 2 SP - 917 EP - 927 PB - Wiley Periodicals LLC AN - OPUS4-51597 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, Ralf A1 - Rabe, Torsten T1 - Improved thermoelectric properties of CaMnO3 and Ca3Co4O9 by increasing the driving force for sintering N2 - Thermoelectric materials can convert waste heat directly into electrical power by utilizing the Seebeck effect. Calcium cobaltite (Ca3Co4O9, p-type) and calcium manganate (CaMnO3, n-type) are two of the most promising oxide thermoelectric materials. The performance of these materials is evaluated by the power factor PF = S²∙σ and the figure of merit ZT = (PF ∙ T) / κ, demanding high Seebeck coefficient S, high electrical conductivity σ and low thermal conductivity κ. The latter two are increasing with increasing relative sinter density. According to theory, the relative density of ceramics can be improved by increasing the driving force for sintering. This study investigates different approaches to increase the driving force for sintering of Ca3Co4O9 and CaMnO3 to improve densities and thermoelectric properties. The following approaches were applied: minimizing the energy input during powder synthesis by calcination, fine milling of the powder, using reaction-sintering without a powder synthesis step, and adding a transient liquid phase by sinter additives. All different approaches led to an increased densification and thus higher electrical conductivity and higher PF. Thermal conductivity increased as well but not to the same extent. E.g. reaction-sintering increased the densification of Ca3Co4O9 (p-type) and CaMnO3 (n-type). Consequently, the electrical conductivities improved by about 100 % for both oxides leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Although the thermal conductivity increased as well by 8 %, the figures of merit (ZT) were significantly higher compared to conventionally sintered bars. The addition of 4 wt% CuO as a sinter additive to CaMnO3 lowers the sinter temperature from above 1250 °C to below 1100 °C and increases the relative density. Due to the increased density, both electrical conductivity and PF increased by more than 200 % even though the sintering temperature was 150 K lower. T2 - Electroceramics XVII CY - Online meeting DA - 24.08.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives PY - 2020 AN - OPUS4-51163 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bresch, Sophie A1 - Mieller, Björn A1 - Moos, Ralf A1 - Rabe, Torsten T1 - Reaction sintering and sintering additives for cost-effective production of thermoelectric oxides N2 - Thermoelectric oxides attract much interest recently. Although their thermoelectric properties are inferior to non-oxides, they exhibit distinct advantages. Thermoelectric oxides are stable in air at higher temperatures, their raw materials are less toxic, and more abundant. To enhance attractivity of these materials for industrial applications, production costs need to be reduced. Conventionally, the legs of thermoelectric generators are sintered from green bodies of previously synthesized powder. Reaction-sintering is a fabrication method without a powder synthesis step, as the final phase is formed during the sintering from a raw material mixture. Moreover, the reduction of chemical potential during reaction-sintering is effective as an additional driving force for sintering. We show that reaction-sintering increases the densification of CaMnO3 (n-type, Sm doped). Consequently, the electrical conductivities improved by about 100 % leading to superior power factors (PF = 230 µW/mK² for CaMnO3). Another approach to reduce the production costs is to lower the sintering temperature by adding sinter additives. The addition of 4 wt% CuO to CaMnO3 lowers the sinter temperature from 1250 °C to 1050 °C. The achieved power factor PF = 264 µW/mK is more than two times higher as reported in literature for the same dopant. T2 - Virtual Conference on Thermoelectrics (VCT) CY - Online meeting DA - 21.07.2020 KW - Thermoelectrics KW - Reaction sintering KW - Sintering additives KW - Calcium manganate KW - Calcium cobaltite PY - 2020 AN - OPUS4-51070 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Sonnenburg, Elke A1 - Bettge, Dirk A1 - Sommer, Kontantin A1 - Agudo Jácome, Leonardo T1 - Präparation, Kontrastierung und Darstellung des Gefüges von additiv gefertigtem austenitischem Stahl 316L N2 - Der weit verbreitete austenitische Stahl 316L soll auch mittels additiver Fertigung verarbeitet werden (316L-AM). Zur Entwicklung optimaler Aufbauverfahren ist ein detailliertes Verständnis des Gefüges notwendig. Das additiv aufgebaute Gefüge zeigt eine Mikrostruktur, die geprägt ist von sehr hohen Abkühlraten und gerichtetem Kornwachstum. Mittels klassischer Metallographie können die Charakteristika des Gefüges wie Körner, Subkörner und Schmelzlinien sichtbar gemacht werden. Mittels EBSD werden Kristallorientierungen ermittelt und bildhaft aufbereitet. Die Feinstruktur der Körner wird im REM in der Übersicht aufgelöst. Erst im TEM kann bei hoher Vergrößerung die Natur der Zellstruktur quantitativ ermittelt werden. T2 - Metallographie 2020 CY - Online meeting DA - 16.09.2020 KW - Präparation KW - Kontrastierung KW - Additiv gefertigter Stahl PY - 2020 AN - OPUS4-51245 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Herzel, Hannes T1 - Phase reaction during thermochemical treatment of sewage sludge and biomass ashes with alkali compounds to increase nutrient plant availability N2 - Das Element Phosphor ist für Pflanzen, Tiere und Menschen essenziell. Um die Phosphorversorgung für Pflanzen in der Landwirtschaft zu gewährleisten, werden Phosphordünger eingesetzt. Die Nährstoffe werden hauptsächlich durch Wirtschaftsdünger (Gülle, Jauche, Stallmist) zurückgeführt. Zusätzlich werden in der konventionellen Landwirtschaft mineralische Phosphordünger eingesetzt, die vorwiegend aus dem fossilen Rohstoff Phosphorit gewonnen werden. Um die Abhängigkeit von fossilen Rohstoffen zu reduzieren, sollen nährstoffhaltige Rest- und Abfallstoffe zur Phosphordünger aufbereitet werden. In Abwasserkläranlagen fällt phosphorreicher Klärschlamm als Abfallstoff an. Der größte Anteil des Klärschlammes wird in Steinkohlekraftwerken, Zementwerken oder in Monoklärschlammverbrennungsanlagen verbrannt. Die Klärschlammaschen aus den Monoverbrennungsanlagen enthalten bis zu 12 Gew.-% Phosphor und sind daher für die Düngerherstellung geeignet. Ein geeignetes Verfahren zur Aufbereitung der Klärschlammaschen ist die thermochemische Behandlung im Drehrohrofen. Mit dem sogenannten AshDec®-Prozess, kann ein Phosphordünger hergestellt werden. Aktuell wird eine großtechnische Anlage in Altenstadt (Bayern) geplant, die im Jahr 2023 den Betrieb aufnehmen soll. Der zentrale Bestandteil ist die Phasenumwandlung von schlecht pflanzenverfügbaren Phosphaten in der Klärschlammasche (vorwiegend das Calciumphosphat Whitlockit und Aluminiumphosphat) zu gut pflanzenverfügbaren Calciumalkaliphosphaten im Produkt. Um dies zu erzielen, werden die Aschen mit Natrium- und/oder Kalium-Verbindungen gemischt und einer thermochemischen Behandlung bei 800-1000 °C zugeführt. Um die Pflanzenverfügbarkeit und Düngewirkung von Phosphaten abschätzen zu können, ist die chemische Extraktionsmethode mit neutraler Ammoniumcitratlösung geeignet. In der Dissertation werden die (Phosphor-)Phasenreaktionen und die Prozessbedingungen des thermochemischen Verfahrens untersucht, um das Verfahren gezielt zu modifizieren und die Wirtschaftlichkeit zu steigern. Die Zielphasen der thermochemischen Behandlung sind die Calciumalkaliphosphate CaNaPO4 und CaKPO4, und deren Mischphasen Ca(Na,K)PO4, welche in der Publikation 3.1 synthetisiert wurden. Für diese Calciumalkaliphosphate wurden die thermodynamischen Daten der Standardbildungsenthalpie, Standardentropie, Wärmekapazität und die Wärmemenge der Phasenumwandlung bestimmt (Publikation 3.1). Bei der thermochemischen Behandlung von Klärschlammaschen wurden als Additive Natrium- und Kaliumsulfat bei verschiedenen Temperaturen getestet. Der Einsatz von Kaliumadditiven ist erwünscht, um den Marktwert des Produktes durch die Produktion eines Phosphor-Kalium-Düngers zu erhöhen. Zusätzlich wird eine möglichst geringe Prozesstemperatur angestrebt, bei der die erwünschten Calciumalkaliphosphate gebildet werden. In den Publikationen 3.2 und 3.3 wird gezeigt, dass für Klärschlammaschen eine komplette Phasenumwandlung zu Calciumnatriumphosphaten ab 875 °C in Laborversuchen (Korundtiegel) mit dem Additiv Natriumsulfat erzielt werden kann. Der Einsatz von Kaliumsulfat erforderte notwendige Reaktionstemperaturen von über 1100 °C. Diese unterschiedlichen Reaktionstemperaturen hängen mit den Schmelzpunkten von Natriumsulfat (890 °C) und Kaliumsulfat (1070 °C) zusammen. Um Kaliumsulfat in den Prozess bei niedrigen Temperaturen zu integrieren, wurden Natriumsulfat und Kaliumsulfat vor der Behandlung gemischt. Dies führte zu einer Schmelzpunkterniedrigung und resultierte in Reaktionstemperaturen zwischen 900 °C bis 1000 °C für die untersuchten Mischungen von Natrium- und Kaliumsulfat (Publikation 3.3). Die Zusammensetzung der Calciumalkaliphosphate Ca(Na,K)PO4 war anders als erwartet. Bei der Phasenanalytik stellte sich heraus, dass bei geringem und mittlerem Anteil von Kaliumsulfat im Alkali-Additiv nur Calciumnatriumphosphate mit sehr geringen Kaliumgehalten gebildet wurden. Erst bei einem hohen Anteil von Kaliumsulfat in der Mischung der Alkalisulfate konnten kaliumhaltige Calciumalkaliphosphate nachgewiesen werden (u.a. (Ca0.9Mg0.1)(Na0.6K0.4)PO4). Dieser geringere Einbau von Kalium in die Calciumalkaliphosphate hängt mit den zusätzlich stattfindenden Reaktionen zwischen den Alkalien und den Silikaten zusammen. Es ist bekannt, dass die zugegebenen Alkalisulfate zuerst mit Silikaten und anschließend mit den Phosphaten reagieren. Silikate bauen bevorzugt Kalium ein, deswegen konnten erst kaliumhaltige Phosphate gebildet werden, wenn die Reaktion mit den Silikaten abgeschlossen war. Dies führte zu einem geringeren Kaliumanteil in den gebildeten Phosphaten im Vergleich zum Kaliumanteil der verwendeten Alkaliadditive. Das in Silikaten gebundene Kalium ist wahrscheinlich schlecht für die Pflanzen verfügbar. Dies könnte den Einsatz der produzierten Phosphor-Kalium-Dünger einschränken. Der bevorzugte Kaliumeinbau in Silikaten konnte auch in Kalkulationen mit den thermodynamischen Daten aus der Publikation 3.1 gezeigt werden. Mittels Phasenanalytik vor und nach der chemischen Extraktion, konnte die Zugehörigkeit zu verschiedenen Modifikationen der Calciumalkaliphosphaten sicher bestimmt werden und eine ungefähre Zusammensetzung dieser Calciumalkaliphosphate abgeschätzt werden. So konnte nachgewiesen werden, dass die Modifikation vom CaNaPO4 ungefähr 10 % Magnesium einbauen kann. Wenn mehr Magnesium eingebaut wird, bildet sich die Phase (Ca,Mg)NaPO4, die eine vergleichbare Struktur wie die bekannte Phase (Ca0.72Mg0.28)NaPO4 aufweist. Dieses magnesiumreiche Calciumnatriumphosphat entstand vermutlich, wenn entweder erhöhte Anteile an Kalium eingebaut wurden (Ca0.8Mg0.2)(Na0.85K0.15)PO4 (Publikation 3.3) oder die Phasenumwandlung vom Calciumphosphat Whitlockit zum Calciumalkaliphosphat CaNaPO4 noch nicht abgeschlossen war (Publikation 3.2). Wenn mehr Kalium eingebaut wird, dann entsteht eine Phase (u.a. (Ca0.9Mg0.1)(Na0.6K0.4)PO4) ähnlich zu den Mischphasen aus der Publikation 3.1. In den Publikationen 3.4 und 3.5 wurden keine Klärschlammaschen untersucht, sondern Biokohlen aus Modellklärschlämmen (Publikation 3.5) und Biomasseaschen (Publikation 3.4) aus der Vergasung oder Verbrennung einer Mischung aus Zuckerrohrbagasse und Hühnertrockenkot. Die thermochemischen Produkte der Biokohlen bzw. Biomasseaschen enthielten das gewünschte CaNaPO4 und hatten eine hohe Düngewirkung in Pflanzenwachstumsversuchen mit Sojapflanzen bzw. Gräsern. KW - AshDec KW - Recycling fertilizer KW - Calcium alkali phosphate PY - 2020 SP - 1 EP - 186 CY - Jena AN - OPUS4-54724 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fortini, Renata A1 - Meyer-Plath, A. A1 - Kehren, D. A1 - Gernert, U. A1 - Agudo Jácome, Leonardo A1 - Sturm, Heinz T1 - Measurement of flexural rigidity of multi-walled carbon nanotubes by Dynamic Scanning Electron Microscopy N2 - In this work the flexural rigidity of individual large diameter multi-walled carbon nanotubes (MWCNTs) was investigated. The bending modulus were obtained by detecting the resonance frequencies of mechanically excited cantilevered carbon nanotubes using the so-called dynamic scanning electron microscopy technique, and applying the Euler–Bernoulli beam theory. For the nanotubes studied, we determined a modulus of up to 160 GPa. This agrees with values reported by other authors for MWCNTs produced by catalytic chemical vapor deposition, however, it is 6-8 times smaller than values reported for single and multi-walled carbon nanotubes produced by arc-discharge synthesis. Toxicological studies with carbon nanotubes have been showing that inhaled airborne nanofibers that reach the deep airways of the respiratory system may lead to serious, asbestos-like lung diseases. These studies suggested that their toxicity critically depends on the fiber flexural rigidity, with high rigidity causing cell lesions. To complement the correlation between observed toxicological effects and fiber rigidities, reliable and routinely applicable measurement techniques for the flexural rigidity of nanofibers are required. KW - Flexural rigidity KW - Bending modulus KW - Resonance frequency KW - Carbon nanotubes KW - Fiber toxicology PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-514190 DO - https://doi.org/10.3390/fib8050031 SN - 2079-6439 VL - 8 IS - 5 SP - 31 PB - MDPI AN - OPUS4-51419 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tomiak, F. A1 - Schartel, Bernhard A1 - Wolf, M. A1 - Drummer, D. T1 - Particle Size Related Effects of Multi-Component Flame-Retardant Systems in poly(butadiene terephthalate) N2 - Aluminum tris (diethylphosphinate) (AlPi) is known to have an efficient flame-retardant effect when used in poly(butadiene terephthalates) (PBT). Additionally, better flame-retardant effects can be achieved through the partial substitution of AlPi by boehmite in multi-component systems, which have been shown to be an effective synergist due to cooling effects and residue formation. Although the potential of beneficial effects is generally well known, the influence of particle sizes and behavior in synergistic compositions are still unknown. Within this paper, it is shown that the synergistic effects in flammability measured by limiting oxygen index (LOI) can vary depending on the particle size distribution used in PBT. In conducting thermogravimetric analysis (TGA) measurements, it was observed that smaller boehmite particles result in slightly increased char yields, most probably due to increased reactivity of the metal oxides formed, and they react slightly earlier than larger boehmite particles. This leads to an earlier release of water into the system enhancing the hydrolysis of PBT. Supported by Fourier transformation infrared spectroscopy (FTIR), we propose that the later reactions of the larger boehmite particles decrease the portion of highly flammable tetrahydrofuran in the gas phase within early burning stages. Therefore, the LOI index increased by 4 vol.% when lager boehmite particles were used for the synergistic mixture. KW - Flame retardants KW - Aluminum diethylphosphinate KW - Boehmite KW - Poly(butadiene terephthalates) (PBT) KW - Mechanical properties PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509286 DO - https://doi.org/10.3390/polym12061315 SN - 2073-4360 VL - 12 IS - 6 SP - 1315 PB - MDPI AN - OPUS4-50928 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Günther, Martin A1 - Levchik, S. V. A1 - Schartel, Bernhard T1 - Bubbles and collapses: Fire phenomena of flame-retarded flexible polyurethane foams N2 - Flexible polyurethane foams (FPUF) are easy to ignite and exhibit rapid flame spread. In this paper, the fire phenomena of two standard foam formulations containing tris (1,3-dichloro-2-propyl) phosphate (FR-2) and a halogen-freepoly (ethyl ethylene phosphate) (PNX), respectively, as flame retardants are compared. A multimethodological approach is proposed which combines standard fire tests as well as new investigatory approaches. The thermophysical properties of the foams were determined by thermogravimetric analysis (TG), reaction to small flames was studied by means of the limiting oxygen index (LOI) and UL 94 HBF test, and the burning behavior was investigated with the cone calorimeter. Further, temperature development in burning cone calorimeter samples was monitored using thermocouples, and rheological measurements were performed on pyrolyzed material, delivering insight into the dripping behavior of the foams. This paper gives comprehensive insight into the fire phenomena of flame-retarded FPUFs that are driven by the two-step decomposition behavior of the foams. LOI and UL 94 HBF tests showed a reduced flammability and reduced tendency to drip for the flame-retarded foams. TG and cone calorimeter measurements revealed that the two-step decomposition behavior causes two stages during combustion, namely structural collapse and pool fire. The flame-retardant mode of action was identified to take place primarily during the foam collapse and be based mainly on flame inhibition. However, some condensed-phase action was been measured, leading to significantly increased melt viscosity and improved dripping behavior for foams containing PNX. KW - Burning behavior KW - Flame retardant KW - Flexible PU foam PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-512145 DO - https://doi.org/10.1002/pat.4939 SN - 1042-7147 SN - 1099-1581 VL - 31 IS - 10 SP - 2185 EP - 2198 PB - Wiley Online Libary AN - OPUS4-51214 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pu, Y. A1 - Lawrence, M. J. A1 - Celorrio, V. A1 - Wang, Q. A1 - Gu, M. A1 - Sun, Z. A1 - Agudo Jácome, Leonardo A1 - Russell, A. E. A1 - Huang, L. A1 - Rodriguez, P. T1 - Nickel confined in 2D earth-abundant oxide layers for highly efficient and durable oxygen evolution catalysts N2 - Low cost, high-efficiency catalysts towards water splitting are urgently required to fulfil the increasing demand for energy. In this work, low-loading (<20 wt%) Ni-confined in layered metal oxide anode catalysts (birnessite and lepidocrocite titanate) have been synthesized by facile ion exchange methodology and subjected to systematic electrochemical studies. It was found that Ni-intercalated on K-rich birnessite (Ni-KMO) presents an onset overpotential (ηonset) as low as 100 mV and overpotential at 10 mA cm−2 (η10) of 206 mV in pH = 14 electrolyte. By combining electrochemical methods and X-ray absorption and emission spectroscopies (XAS and XES), we demonstrate Ni sites are the active sites for OER catalysis and that the Mn3+ sites facilitate Ni intercalation during the ion-exchange process, but display no observable contribution towards OER activity. The effect of the pH and the nature of the supporting electrolyte on the electrochemical performance was also evaluated. KW - Confined catalyst KW - Low-loading KW - Layered manganese oxide KW - Oxygen evolution reaction KW - Transmission electron microscopy (TEM) PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515027 DO - https://doi.org/10.1039/D0TA04031B SN - 2050-7496 SN - 2050-7488 VL - 8 IS - 26 SP - 13340 EP - 13350 PB - Royal Society of Chemistry CY - London AN - OPUS4-51502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg T1 - Reductive Defluorination and Mechanochemical Decomposition of Per- and Polyfluoroalkyl Substances (PFASs): From Present Knowledge to Future Remediation Concepts N2 - Over the past two decades, per- and polyfluoroalkyl substances (PFASs) have emerged as worldwide environmental contaminants, calling out for sophisticated treatment, decomposition and remediation strategies. In order to mineralize PFAS pollutants, the incineration of contaminated material is a state-of-the-art process, but more cost-effective and sustainable technologies are inevitable for the future. Within this review, various methods for the reductive defluorination of PFASs were inspected. In addition to this, the role of mechanochemistry is highlighted with regard to its major potential in reductive defluorination reactions and degradation of pollutants. In order to get a comprehensive understanding of the involved reactions, their mechanistic pathways are pointed out. Comparisons between existing PFAS decomposition reactions and reductive approaches are discussed in detail, regarding their applicability in possible remediation processes. This article provides a solid overview of the most recent research methods and offers guidelines for future research directions. KW - PFAS KW - Reductive defluorination KW - Reductive decomposition KW - Mechanochemistry KW - Remediation PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513811 DO - https://doi.org/10.3390/ijerph17197242 VL - 17 IS - 19 SP - 1 EP - 22 PB - MDPI AG CY - Basel AN - OPUS4-51381 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Wiesler, F. A1 - Hund-Rinke, K. A1 - George, E. A1 - Greef, J.-M. A1 - Holz, F. A1 - Hölze, L.E. A1 - Hülsbergen, K.-J. A1 - Martin, S. A1 - Severin, K. A1 - Spielvogel, S. A1 - Geiger, P. A1 - Nawotke, C. A1 - Kehlenbeck, H. A1 - Schenkel, H. A1 - Adam, Christian A1 - Bloem, E. A1 - Frank, D. A1 - Goldbach, H.E. A1 - Heene, M. A1 - Kratz, S. A1 - Kruse, A. A1 - Möller, K. A1 - Pinnekamp, J. A1 - Schoumans, O.F. A1 - Vogel, Christian A1 - Wulf, S. T1 - Recyclingphosphate in der Düngung – Nutzen und Grenzen N2 - Weltweit werden etwa 80–85 % aller abgebauten Rohphosphate für die Produktion von Düngemitteln verwendet. Bei noch steigendem Bedarf an Phosphor (P) geht man derzeit davon aus, dass die weltweiten P-Reserven noch über 200 Jahre ausreichen. Um den P-Vorrat langfristig abzusichern, sollte der in Reststoffen enthaltene Phosphor möglichst umfänglich genutzt werden. Dieser Forderung trägt das von der Bundesregierung 2012 erstmals beschlossene Deutsche Ressourceneffizienzprogramm ProgRess Rechnung. Rohphosphat wird auch seitens der Europäischen Kommission aufgrundseiner ökonomischen Bedeutung und des unsicheren Angebots als „kritischer Rohstoff“ eingestuft. Vor diesem Hintergrund hat die Bundesregierung in der Verordnung zur Neuordnung der Klärschlammverwertung vom 27. September 2017 in Deutschland eine verpflichtende technische Rückgewinnung von Phosphor für Abwasserbehandlungsanlagen ab einer Ausbaugröße von 100.000 Einwohnerwerten (12 Jahre nach Inkrafttreten der Verordnung) bzw. ab einer Ausbaugröße von über 50.000 Einwohnerwerten (15 Jahre nach Inkrafttreten der Verordnung) vorgeschrieben. Die Verordnung enthält keine Vorgaben hinsichtlich der anzuwendenden Technologie bei der Phosphorrückgewinnung. Ausgenommen von der Rückgewinnungspflicht sind Klärschlämme mit niedrigen Phosphorgehalten (weniger als 20 Gramm Phosphor je Kilogramm Klärschlamm-Trockenmasse). Auch die im Jahre 2017 verabschiedeten neuen Rechtsvorschriften für die Düngung verlangen zukünftig einen nachhaltigen und ressourceneffizienten Umgang mit Nährstoffen bei der landwirtschaftlichen Erzeugung und schränken die P-Zufuhr insbesondere auf hoch versorgten Böden ein (Düngeverordnung vom 26. Mai 2017). Dies wird zu einem mehr am Pflanzenbedarf orientierten und ggf. vermehrt überbetrieblichen Einsatz von wirtschaftseigenen Düngern führen. Um den politischen und gesetzlichen Anforderungen gerecht zu werden, müssen einerseits wirksame und kosteneffiziente technische Verfahren zum P-Recycling (weiter)entwickelt werden. Andererseits müssen die Recyclingprodukte die Anforderungen für eine direkte Verwendung in der Landwirtschaft oder als Rohstoff für die Herstellung von Düngemitteln erfüllen. In dem vorliegenden Standpunkt wird zunächst der potenzielle Beitrag von Reststoffen zur Deckung des P-Bedarfs in der deutschen Pflanzenproduktion geschätzt. Für die wichtigsten Reststoffe werden technische Verfahren zur P-Rückgewinnung bzw. Aufarbeitung skizziert. Auf Basis der Anforderungen der Landwirtschaft bzw. der Düngemittelindustrie an die P-Recyclingprodukte werden deren Herstellungsverfahren bewertet. Schließlich wird der Regelungs- und Forschungsbedarf formuliert. KW - Phosphor KW - Düngemittel KW - Diffusive Gradients in thin films (DGT) PY - 2020 SP - 1 EP - 19 PB - Bundesministerium für Ernährung und Landwirtschaft (BMEL) CY - Berlin AN - OPUS4-51011 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gehrenkemper, Lennart A1 - Simon, Fabian A1 - Roesch, Philipp A1 - Fischer, E. A1 - von der Au, Marcus A1 - Pfeifer, Jens A1 - Cossmer, Antje A1 - Wittwer, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg A1 - Meermann, Björn T1 - Determination of organically bound fluorine sum parameters in river water samples - Comparison of combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) N2 - In this study, we compare combustion ion chromatography (CIC) and high resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) with respect to their applicability for determining organically Bound fluorine sum parameters. Extractable (EOF) and adsorbable (AOF) organically bound fluorine as well as total fluorine (TF) were measured in samples fromriver Spree in Berlin, Germany, to reveal the advantages and disadvantages of the two techniques used as well as the two established fluorine sum Parameters AOF and EOF. TF concentrations determined via HR-CS-GFMAS and CIC were comparable between 148 and 270 μg/L. On average, AOF concentrations were higher than EOF concentrations, with AOF making up 0.14–0.81% of TF (determined using CIC) and EOF 0.04–0.28% of TF (determined using HR-CSGFMAS). The results obtained by the two independent methods were in good agreement. It turned out that HR-CS-GFMAS is a more sensitive and precise method for fluorine analysis compared to CIC. EOF and AOF are comparable tools in Risk evaluation for the emerging pollutants per- and polyfluorinated alkyl substances; however, EOF is much faster to conduct. KW - High resolution-continuum source-graphite furnace molecular absorption spectrometry (HR-CS-GFMAS) KW - Combustion ion chromatography (CIC) KW - Per- and polyfluorinated alkyl substances (PFASs) KW - Adsorbable organically bound fluorine (AOF) KW - Extractable organically bound fluorine (EOF) KW - Surface waters PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-515351 DO - https://doi.org/10.1007/s00216-020-03010-y SN - 1618-2650 VL - 413 IS - 28 SP - 103 EP - 115 PB - Springer CY - Berlin AN - OPUS4-51535 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Sekine, R. A1 - Huang, J. A1 - Steckenmesser, D. A1 - Steffens, D. A1 - Huthwelker, T. A1 - Borca, C. A1 - Pradas del Real, A. A1 - Castillo-Michel, H. A1 - Adam, Christian T1 - Effects of a nitrification inhibitor on nitrogen species in the soil and the yield and phosphorus uptake of maize N2 - Phosphorus (P) resource availability is declining and the efficiency of applied nutrients in agricultural soils is becoming increasingly important. This is especially true for P fertilizers from recycled materials, which often have low plant availability. Specific co-fertilization with ammoniumcan enhance P plant availability in soils amended with these P fertilizers, and thus the yield of plants. To investigate this effect, we performed a pot experiment with maize in slightly acidic soil (pH 6.9) with one water-soluble (triple superphosphate [TSP]) and two water-insoluble (sewage sludge-based and hyperphosphate [Hyp]) P fertilizers and anammoniumsulfate nitrate with or without a nitrification inhibitor (NI). The dry matter yield of maize was significantly increased by the NI with the Hyp (from 14.7 to 21.5 g/pot) and TSP (from 40.0 to 45.4 g/pot) treatments. Furthermore, P uptake was slightly increased in all three P treatments with the NI, but not significantly. Olsen-P extraction and P K-edge micro-X-ray absorption near-edge structure (XANES) spectroscopy showed that apatite-P of the water insoluble P fertilizers mobilized during the plant growth period. In addition, novel nitrogen (N) K-edge micro-XANES spectroscopy and the Mogilevkina method showed that the application of an NI increased the fixation of ammonium in detectable hot spots in the soil. Thus, the delay in the nitrification process by the NI and the possible slow-release of temporarily fixed ammoniumin the soil resulted in a high amount of plant available Ammonium in the soil solution. This development probably decreases the rhizosphere pH due to release of H+ by plants during ammoniumuptake, whichmobilizes phosphorus in the amended soil and increases the dry matter yield of maize. This is especially important for water-insoluble apatite-based P fertilizers (conventional and recycled), which tend to have poor plant availability. KW - Fertilzer KW - Phosphorus recovery KW - Ammonium KW - Nitrification inhibitor KW - XANES spectroscopy KW - Diffusive gradients in thin films (DGT) PY - 2020 DO - https://doi.org/10.1016/j.scitotenv.2020.136895 SN - 1879-1026 VL - 715 SP - 1 EP - 8 PB - Elsevier CY - Amsterdam AN - OPUS4-50477 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Hoffmann, Marie A1 - Krüger, O. A1 - Murzin, V. A1 - Caliebe, W. A1 - Adam, Christian T1 - Chromium (VI) in phosphorus fertilizers determined with the diffusive gradients in thin-films (DGT) technique N2 - Phosphorus (P) fertilizers from secondary resources became increasingly important in the last years. However, these novel P-fertilizers can also contain toxic pollutants such as chromium in its hexavalent state (Cr(VI)). This hazardous form of chromium is therefore regulated with low limit values for agricultural products even though the correct determination of Cr(VI) in these fertilizers may be hampered by redox processes, leading to false results. Thus, we applied the novel diffusive gradients in thin-films (DGT) technique for Cr(VI) in fertilizers and compared the results with the standard wet chemical extraction method (German norm DIN EN 15192) and Cr K-edge X-ray Absorption near-edge structure (XANES) spectroscopy. We determined an overall good correlation between the wet chemical extraction and the DGT method. DGT was very sensitive and for most tested materials selective for the analysis of Cr(VI) in P-fertilizers. However, hardly soluble Cr(VI) compounds cannot be detected with the DGT method since only mobile Cr(VI) is analyzed. Furthermore, Cr K-edge XANES spectroscopy showed that the DGT binding layer also adsorbs small amounts of mobile Cr(III) so that Cr(VI) values are overestimated. Since certain types of the P fertilizers contain mobile Cr(III) or partly immobile Cr(VI), it is necessary to optimize the DGT binding layers to avoid aforementioned over- or underestimation. Furthermore, our investigations showed that the Cr K-edge XANES spectroscopy technique is unsuitable to determine small amounts of Cr(VI) in fertilizers (below approx. 1% of Cr(VI) in relation to total Cr). KW - Phosphorus fertilizer KW - Sewage sludge ash KW - Diffusive Gradients in thin films (DGT) KW - Chemical extraction KW - XANES spectroscopy PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-509578 DO - https://doi.org/10.1007/s11356-020-08761-w SN - 0944-1344 VL - 27 SP - 24320 EP - 24328 PB - Springer AN - OPUS4-50957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gentzmann, Marie A1 - Adam, Christian A1 - Vogel, Christian A1 - Gäbler, H.-E. A1 - Huthwelker, T. T1 - Investigation and comparison of Scandium species in different European bauxite residues by combination of novel analytocall tools N2 - In recent times, as the need for new high-tech materials is growing steadily to fulfil future sustainability goals, more and more looks turn towards industrial waste streams as potential sources of valuable metals. Bauxite residue (BR), accumulating during alumina production, is one of the major waste streams in the metal industry. Suitable re-use possibilities for BR are intensively investigated including approaches for the recovery of scandium (Sc). This transition metal, even though rarely recognized by the broader audience yet, has recently gained the interest of e.g. aerospace industries and SOFC-producers since its use is strongly improving the performance and durability of the respective materials. Even though many sources classify Sc as one of the REE, there are many aspects, such as its ionic radius, which significantly differentiate Sc from the REE and cause its behaviour to be distinct as well. The large ionic potential (radius/charge) causes Sc to be incompatible in most rock forming minerals, which results in generally low concentrations in the earth’s crust and rare occurrences of natural Sc-deposits. The general occurrence of enriched concentrations of Sc in some BRs compared to the earth’s crust is known for some time now and has especially been investigated for Greek materials. However, the (geo)chemical and mineralogical behaviour, the Sc speciation, the association and the variation of Sc occurrences in BRs of different origin is still not fully understood. This study aims to gain better knowledge on the different kinds of Sc-occurrences and their possible impact on future recovery schemes. We therefore apply a diverse set of analytical methods including novel measurement techniques such as X-ray absorption near edge structure (XANES) spectroscopy as well as standard techniques such as electron microprobe analyses, and Raman spectroscopy on BRs from Germany, Hungary and Greece. Information on the local distribution of Sc is determined by high-resolution laser ablation – inductively coupled plasma – mass spectrometry (LA-ICP-MS) mappings. Sc in Greek BR seems to have an affinity towards Fe-Phases such as Goethite and Hematite. However, whereas some of these phases show distinct enrichment of Sc, others are particularly barren, which might be a result of the different input materials. By means of XANES measurements it was possible to show that Sc in the Greek samples occurs adsorbed on the surface of those Fe-Phases, likely in the form of amorphous Sc-hydroxide or -oxyhydroxide or can be incorporated into the crystal lattice as well. The general affinity of Sc to those kinds of phases has been reported for natural rocks such as laterites before, where similar investigations were made using the XANES method [8]. Likewise, the Fe-association has been observed for Greek BR by Vind et al. [7]. Hungarian BRs show similar results as the Greek samples and LA-ICP-MS mappings show distinct Sc enrichment rims surrounding mineral particles. In German BR, Fe as well as Ti-phases occur to be partially enriched in Sc. Depending on the original primary bauxite, the source rock of the bauxite and the bauxite processing route, it is likely that many different parameters influence the occurrence and species of Sc in the BR. Theoretically, it either can therefore remain within its original carrier or can be partially or fully redistributed within the BR. Since the processing of the bauxite involves elevated temperatures, pressure and dissolving reagents, it is however very likely that some of the Sc will be redistributed and adsorb on mineral surfaces of smaller and larger particles, making beneficiation steps rather ineffective. The study shows that there is no general rule defining how Sc is associated mineralogically or chemically within BRs. Therefore, the effective development of a recovery method needs a case specific background knowledge on the Sc-species present in the BR of interest. This research has received funding from the European Community’s Horizon 2020 Programme SCALE (H2020/2014-2020) under grant agreement n° 730105. T2 - 3rd European Rare Earth Resources Conference (ERES) 2020 CY - Online meeting DA - 06.10.2020 KW - Red Mud KW - Scandium KW - Bauxite Residue PY - 2020 AN - OPUS4-51570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Roesch, Philipp A1 - Vogel, Christian A1 - Simon, Franz-Georg T1 - 8. Netzwerktreffen PerFluSan N2 - Vorstellung der Projektarbeit der BAM auf dem 8. Netzwerktreffen PerFluSan in Dresden T2 - 8. Netzwerktreffen PerFluSan CY - Fraunhofer IKTS, Dresden, Germany DA - 09.03.2020 KW - PFC KW - Sanierung KW - Kontamination KW - Boden PY - 2020 AN - OPUS4-50552 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Straub, D. A1 - Schneider, Ronald A1 - Bismut, E. A1 - Kim, H.-J. T1 - Reliability analysis of deteriorating structural systems N2 - Reliability analysis of deteriorating structural systems requires the solution of time-variant reliability problems. In the general case, both the capacity of and the loads on the structure vary with time. This analysis can be approached by approximation through a series of time-invariant reliability problems, which is a potentially effective strategy for cases where direct solutions of the time-variant reliability problem are challenging, e.g. for structural systems with many elements or arbitrary load processes. In this contribution, we thoroughly Review the formulation of the equivalent time-invariant reliability problems and extend this approximation to structures for which inspection and monitoring data is available. Thereafter, we present methods for efficiently evaluating the reliability over time. In particular, we propose the combination of sampling-based methods with a FORM (first-order reliability method) approximation of the series system reliability problem that arises in the computation of the lifetime reliability. The framework and algorithms are demonstrated on a set of numerical examples, which include the computation of the reliability conditional on inspection data. KW - Monitoring KW - Reliability KW - Deterioration KW - Structural systems KW - Bayesian analysis KW - Inspection PY - 2020 DO - https://doi.org/10.1016/j.strusafe.2019.101877 VL - 82 SP - Paper 101877, 1 PB - Elsevier Ltd. AN - OPUS4-48952 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Adam, Christian A1 - Herzel, Hannes T1 - Modifiziertes Rhenania Phosphat auf Klärschlammasche für Bayern N2 - Es wurde das Projekt R-Rhenania MODIFIZIERTES RHENANIA PHOSPHAT AUS KLÄRSCHLAMMASCHE FÜR BAYERN mit seinen Inhalten und der Projektstruktur vorgestellt. T2 - 6. P-Rück-Kongress: Phosphor - ein kritischer Rohstoff mit Zukunft CY - Online meeting DA - 25.11.2020 KW - Phosphorrückgewinnung KW - Klärschlammasche PY - 2020 AN - OPUS4-51667 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolmangadi, Mohamed Aejaz A1 - Szymoniak, Paulina A1 - Smales, Glen Jacob A1 - Alentiev, D. A1 - Bermeshev, M. A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Molecular Dynamics of Janus Polynorbornenes: Glass Transitions and Nanophase Separation N2 - For the first time, dielectric and calorimetric investigations of an homologous series of Janus polynorbornenes with rigid main backbones and flexible -Si(OR)3 side groups, of differing length alkyl chains (R = Propyl, Butyl, Hexyl, Octyl, Decyl) is reported. Generally, this class of polymers has some potential for applications in the field of gas separation membranes. Two dielectrically active processes are observed at low temperatures, denoted as β- and α- relaxation. The former can be assigned to localized fluctuations, whilst the latter is related to the glassy dynamics of the flexible -Si(OR)3 side groups, creating a nanophase separation in both the alkyl chain rich and backbone rich domains. This is confirmed through temperature modulated DSC measurements and X-ray scattering experiments. The glass transition temperatures of the backbone rich domains, which are beyond or near to their degradation temperatures in terms of conventional DSC, are determined for the first time using Fast Scanning Calorimetry employing both fast heating and cooling rates. This is complimented with scattering experiments that show how the size of the alkyl chain rich domains increases with chain length. Alongside these results, a significant conductivity contribution was observed for all poly(tricyclononenes) with -Si(OR)3 side groups, which is interpreted in terms of a percolation model. KW - Polynorbornenes KW - Broadband Dielectric Spectrscopy KW - Advanced calorimetry PY - 2020 DO - https://doi.org/10.1021/acs.macromol.0c01450 VL - 53 IS - 17 SP - 7410 EP - 7419 PB - ACS AN - OPUS4-51196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Schartel, Bernhard A1 - Kebelmann, Katharina ED - Hu, Y. ED - Wang, X. T1 - Fire testing for the development of flame retardant polymeric materials N2 - Flame retarded polymeric materials are used in various applications in which a certain fire behavior is demanded. Protection goals are defined, such as limited flammability in terms of hindered sustained ignition or limited contribution to a fire, and these protection levels are tested with defined specimens or components in defined fire scenarios, that is to say, different fire tests. Passing a specific fire test by meeting whatever its demands is often the most important development goal, so the parameters of the different fire tests vary widely to emphasize different fire properties. Some fire tests are used to screen or provide a general assessment of flame retardant polymers during development, while other fire tests and tailored experiments are performed to address special phenomena or understand the flame retardancy modes of action. For all fire testing, the devil is in the details – demanding know-how and crucial efforts to manage the quality of investigations and advanced interpretation. This chapter aims to offer a structured overview of all these aspects. KW - Fire testing KW - Flame retardant KW - Fire retardant KW - Flammability KW - Ignition KW - Oxygen index KW - Cone calorimeter KW - UL 94 KW - Developing fire KW - Uncertainty KW - Fire resistance PY - 2020 SN - 978-1-138-29578-7 SP - 35 EP - 55 PB - CRC Press AN - OPUS4-50236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Morys, Michael A1 - Häßler, Dustin A1 - Krüger, Simone A1 - Schartel, Bernhard A1 - Hothan, Sascha T1 - Beyond the standard time-temperature curve: Assessment of intumescent coatings under standard and deviant temperature curves N2 - Nowadays there are intumescent coatings available for diverse applications. There is no established assessment of their protection performance besides the standard time-temperature curve, but natural fire scenarios often play an important role. A reliable straightforward performance-based assessment is presented. The effective thermal conductivity per thickness is calculated based on intermediate-scale fire tests. The optimum thermal insulation, the time to reach it, and the time until contingent failure of the coating are used for an assessment independent of the heating curve. The procedure was conducted on four different commercially intumescent coatings for steel construction, one solvent-based, one waterborne, one epoxy-based, and a bandage impregnated with a waterborne coating. The performance was studied under four different but similar shaped heating curves with different maximum temperatures (standard time-temperature curve, hydrocarbon curve and two self-designed curves with reduced temperature). The thermal protection performance is crucially affected by the residue morphology. Therefore, a comprehensive morphology analysis, including micro-computed tomography and scanning electron microscopy, was conducted on small-scale residues (7.5 x 7.5 cm2). Two different types of inner structures and the residue surface after different heat exposures were discussed in terms of their influence on thermal protection performance. KW - Intumescence KW - Coating KW - Computed tomography KW - Small scale KW - Heating curves KW - Residue morphology PY - 2020 DO - https://doi.org/10.1016/j.firesaf.2020.102951 SN - 0379-7112 VL - 112 SP - 102951 PB - Elsevier Ltd. AN - OPUS4-50334 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Turski Silva Diniz, Analice A1 - Huth, Christian A1 - Schartel, Bernhard T1 - Dripping and decomposition under fire: Melamine cyanurate vs. glass fibres in polyamide 6 N2 - Manipulating the melt dripping of thermoplastics makes a fire scenario more or less dangerous. Yet, a detailed understanding of this phenomenon has remained a question mark in studies of the flammability of plastics. In this work, the individual and collective impacts of additives on the dripping behaviour of polyamide 6 (PA6) were studied. A set of materials compounded with melamine cyanurate (MCA) and glass fibre (GF) was investigated. Under UL 94 vertical test conditions, the dripping during first and second ignition was quantified and investigated in detail. The number, size and temperature of the drops were addressed, and the materials and their drops evaluated with respect to such aspects as their averaged molecular weight, thermal decomposition and rheological properties. PA6 with V-2 classification improved to V-0 with the addition of MCA, and achieved HB in the presence of GF. PA6/GF/MCA achieved V-2. Non-flaming drops of PA6/MCA consisted of oligomeric fragments. Flaming drops of PA6/GF showed a more pronounced decomposition of PA6 and an increased GF content. The dripping behaviour of PA6/GF/MCA can be understood as a combination of the influence of both additives. The results showed nicely that dripping under fire is neither a straightforward material property nor a simple additive influence, but the complex response of the material influenced by the interaction and competition of different phenomena. KW - Dripping KW - UL 94 KW - Polyamide 6 KW - Melamine cyanurate KW - Glass fibre KW - Flame retardant PY - 2020 DO - https://doi.org/10.1016/j.polymdegradstab.2019.109048 SN - 0141-3910 VL - 171 SP - 109048 PB - Elsevier Ltd. AN - OPUS4-50239 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen A1 - Falkenhagen, Jana A1 - Kricheldorf, H. T1 - Polymer mass spectrometry at BAM with special emphasis on MALDI and ESI N2 - Since its introduction mass spectrometric techniques like Matrix-assisted Laser Desorption/ionization (MALDI) and Electrospray Ionization (ESI) have become indispensable for synthetic polymer analyses. Ideally, various polymer properties (monomer structure, masses, mass distribution, end groups) can be determined simultaneously. However, in real life these experiments are always affected by important structural parameters and instrumental limitations. A short introduction focussing on latest findings with respect to ionisation principles and mechanisms will be given. Recent results from our group will be presented and efforts to avoid common drawbacks of polymer mass spectrometry will be discussed. In this regard, MALDI - Imaging mass spectrometry and the 2D hyphenation of MS with different chromatographic separation techniques were especially useful, since they can provide additional information and reduce the complexity of polymer analyses. T2 - 21. European Symposium on Polymer Spectroscopy CY - Linz, Austria DA - 13.01.2020 KW - Mass spectrometry KW - MALDI-TOF MS KW - ESI-TOF MS KW - Polymer PY - 2020 AN - OPUS4-50260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schartel, Bernhard T1 - Flammschutz für technische Kunststoffte für elektronische Anwendungen N2 - Das Brandverhalten stellt wie das ausgezeichnete elektrische Isolationsverhalten, die geringen elektrischen Verluste, die Verarbeitbarkeit und Formbarkeit eine der wesentlichen Schlüsseleigenschaften im Eigenschaftsprofil von Polymerwerkstoffen in der Elektronik und der Elektrotechnik dar. Dabei bedarf es einer Ausrüstung der Polymerwerkstoffe mit Flammschutzmittel. Die Entwicklung von immer effizienteren, synergistischen und multifunktionalen Multikomponentensystemen ist dabei eine herausragende Quelle für Innovation. Die Entwicklung und Verbesserung der werkstoff- und anwendungsspezifischen Flammschutzlösungen bestimmen die aktuellen und zukünftigen Polymermaterialien in der Elektronik und Elektrotechnik mit. Der Vortrag stellt anhand von Beispielen einige der erfolgreichen Konzepte dar. Es wird versucht, über das wissenschaftlich-systematische Verständnis Grundprinzipien und vielversprechende Lösungsstrategien zu verdeutlichen. T2 - Kunststoff trifft Elektronik, KUZ Kunststoffzentrum in Leipzig CY - Leipzig, Germany DA - 29.01.2020 KW - Flame retardant KW - Ssynergy KW - Flame retardant mode of action KW - UL 94 KW - Cone calorimeter PY - 2020 AN - OPUS4-50495 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - López-Galilea, I. A1 - Ruttert, B. A1 - Theisen, W. A1 - Agudo Jácome, Leonardo T1 - Microstructural characterization of the AlMo 0.5 NbTa 0.5 ZrTi refractory complex concentrated alloy N2 - A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community and the AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. The AlMo0.5NbTa0.5TiZr rCCA was studied by SEM, EDX, EBSD and TEM, showing the presence of a nanoscopic basket-wave structure inside the grains, with two BCC phases. Additionally, thermodynamic calculations on the AlMo0.5NbTa0.5TiZr alloy were done with two different proprietary databases that anticipate two BCC-disordered phases with distinct constitutions as well as an HCP phase. T2 - Symposium on Advanced Mechanical and Microstructural Characterization of High-Entropy Alloys CY - Bochum, Germany DA - 03.02.2020 KW - High Entropy Alloy KW - EBSD KW - Microstructure Characterization PY - 2020 AN - OPUS4-50729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Vogl, Jochen A1 - Rienitz, O. A1 - Rosner, M. A1 - Mieller, Björn A1 - Kasemann, S. A1 - Kraft, R. A1 - Malinovskiy, D. A1 - Meixner, A. A1 - Noordmann, J. A1 - Rabb, S. A1 - Schuessler, J. A. A1 - Vocke, R. D. T1 - Calibration of Mg isotope amount ratios and delta values N2 - In the past, δ26/24Mg measurements were referenced to NIST SRM 980, the initial zero of the δ26/24Mg scale. With the development of MC-ICPMS, the detection of small but measurable isotopic differences in different chips of SRM 980 became apparent. To solve this problem a suite of magnesium isotope reference materials, ERM-AE143, -AE144 and -AE145, has been certified in a first study by applying an ab initio calibration for absolute Mg isotope ratios without any a priori assumptions, a procedure which fulfils all requirements of a primary method of measurement. We could achieve for the first time measurement uncertainties for isotope amount ratios close to the typical precision of magnesium delta values, δ26/24Mg, which are at the 0.1 ‰ level (2SD). In addition, it was demonstrated that commonly used fractionation laws are invalid for correcting Mg isotope ratios in multi-collector ICPMS as they result in a bias which is not covered by its associated uncertainty. Depending on their type, fractionation laws create a bias up to several per mil, with the exponential law showing the smallest bias between 0.1 ‰ to 0.7 ‰. With these isotope reference materials, it is possible to establish SI-traceability for magnesium delta measurements. To realize this, we organized a second study within which five expert laboratories participated to cross-calibrate all available magnesium isotope standards, which are NIST SRM 980, IRMM-009, ERM-AE143, ERM-AE144, ERM-AE145 and the standards DSM3 and Cambridge-1. The mean δ26/24Mg values for the individual iRMs, calculated from the laboratory means show 2 SD reproducibilities varying between 0.025 and 0.093 ‰. Propagated measurement uncertainties suggest a standard uncertainty of about 0.1‰ for δ26/24Mg determinations (2SD). Thus, SI traceability for magnesium isotope amount ratios and delta values is demonstrated to be established. T2 - 53rd annual conference of the DGMS including 27th ICP-MS User's Meeting CY - Münster, Germany DA - 01.03.2020 KW - Isotope ratio KW - Delta value KW - Metrology KW - Magnesium KW - Magnesium isotope ratios PY - 2020 N1 - Geburtsname von Mieller, Björn: Brandt, B. - Birth name of Mieller, Björn: Brandt, B. AN - OPUS4-50549 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hajian, A. A1 - Konegger, T. A1 - Bielecki, K. A1 - Mieller, Björn A1 - Rabe, Torsten A1 - Schwarz, S. A1 - Zellner, C. A1 - Schmid, U. T1 - Wet chemical porosification with phosphate buffer solutions for permittivity reduction of LTCC substrates N2 - The wireless high-frequency technology requires a robust, cost-effective, and highly integrated substrate technology offering the capability for areas of tailored permittivity. The wet-chemical porosification of low temperature co-fired ceramics (LTCC) substrates offers such an approach by locally embedding air. Porosification of LTCC in both extremely acidic and alkaline media has been investigated in previous works. However, for improving the available knowledge on the porosification of LTCC with H3PO4 as a standard and a widely used etching solution, the impact of solution concentration was systematically investigated and a substantial improvement in the etching performance was achieved. Moreover, in the present study, for the first time, the intermediate pH values, and the impact of pH as a key parameter on the etching process have been investigated. For this purpose, the applicability of phosphate buffer solution (PBS) as a prospective novel etchant mixture for the porosification of a commercially available LTCC tape (Ceramtape GC) was explored. Valuable information about surface morphology, crystalline composition, and the pore structure of the etched LTCCs was gathered employing scanning electron microscopy, transmission electron microscopy, X-ray diffraction analysis, and mercury porosimetry measurements. Based on these findings, the performance of PBS-based etchant systems towards the generation of porous LTCCs combining high depths of porosification with acceptable surface characteristics for subsequent metallization is demonstrated. Based on the obtained results, by application of a 0.2 mol L−1 solution of PBS, the effective relative permittivity of test samples with a thickness of approximately 600 µm and a porosification depth of 186 µm from each side, could be reduced up to 10% of its initial “as fired” value. Also, based on the measurement results and by measuring the depth of porosification, the permittivity of the etched layer was estimated to show a reduction of up to 22% compared to the initial “as fired” value. KW - LTCC KW - Porosification KW - Wet chemical etching KW - Permittivity reduction PY - 2020 DO - https://doi.org/10.1016/j.jallcom.2020.158059 SN - 0925-8388 VL - 863 SP - 158059 PB - Elsevier B.V. AN - OPUS4-51800 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana A1 - Epping, Ruben T1 - Microstructure characterization of oligomers by analysis of UPLC / ESI-TOF-MS reconstructed ion chromatograms N2 - It is a well-known story that copolymers beside their molar mass distribution (MMD) can exhibit a functionality type distribution (FTD), a copolymer composition distribution (CCD), a monomer sequence distribution (MSD) and additionally different topologies within one sample. Small, often isobaric heterogeneities in topology or microstructure can usually not be simply separated chromatographically or distinguished by any common detector. Nowadays a wide range of different analytical separation techniques and multi-detection possibilities are available. The challenge consists in a clever combination of these techniques with a specific approach of data analysis. In this presentation different liquid chromatographic separation modes were combined with Electrospray Time-of-Flight mass spectrometry. The online coupling allows the analysis of reconstructed ion chromatograms (RIC) of each degree of polymerization. While a complete separation often cannot be achieved, the derived retention times and peak widths lead to information on the existence and dispersity of heterogeneities in microstructure or topology, that are otherwise inaccessible This method is suitable to detect small differences in e. g. branching, topology, monomer sequence or tacticity and could potentially be used in production control of oligomeric products or other routinely done analyses to quickly indicate deviations from set parameters. Based on a variety of examples e.g. the topology elucidation of branched EO-PO copolymers, the possibilities and limitations of this approach were demonstrated. T2 - Analyticon 2020 CY - Online meeting DA - 05.11.2020 KW - Microstructure KW - Copolymer KW - LC-MS PY - 2020 AN - OPUS4-51540 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ávila Calderón, Luis Alexander A1 - Rehmer, Birgit A1 - Schriever, Sina A1 - Ulbricht, Alexander A1 - Agudo Jácome, Leonardo A1 - Sommer, Konstantin A1 - Mohr, Gunther A1 - Skrotzki, Birgit T1 - Creep and fracture behavior of conventionally and additively manufactured stainless steel 316L N2 - A critical task within the frame of establishing process-structure-property-performance relationships in additive manufacturing (AM) of metals is producing reliable and well-documented material behavior’s data and knowledge regarding the structure-property correlation, including the role of defects. After all, it represents the basis for developing more targeted process optimizations and more reliable predictions of performance in the future. Within this context, this contribution aims to close the actual gap of limited historical data and knowledge concerning the creep behavior of the widely used austenitic stainless steel 316L, manufactured by Laser-Powder-Bed-Fusion (L-PBF). To address this objective, specimens from conventional hot-rolled and AM material were tested under application-relevant conditions according to existing standards for conventional material, and microstructurally characterized before and after failure. The test specimens were machined from single blocks from the AM material. The blocks were manufactured using a standard scan and build-up strategy and were subsequently heat-treated. The creep behavior is described and comparatively assessed based on the creep lifetime and selected creep curves and characteristic values. The effect of defects and microstructure on the material’s behavior is analyzed based on destructive and non-destructive evaluations on selected specimens. The AM material shows shorter creep lives, reaches the secondary creep stage much faster and at a lower strain, and features lower creep ductility compared to its conventional counterpart. The creep damage behavior of the AM material is more microstructure than defect controlled and is characterized by the formation and accumulation of single intergranular damage along the whole volume. Critical features identified are the grain morphology and the grain-boundary as well as the dislocation’s density. Micro-computed tomography (µCT) proves to be an alternative to metallography to analyze the creep damage. T2 - ASTM International Conference on Additive Manufacturing 2020 CY - Online meeting DA - 16.11.2020 KW - 316L KW - Creep behavior KW - Laser powder bed fusion KW - Additive manufacturing KW - Microstructure PY - 2020 AN - OPUS4-51823 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Cornelsen Sampaio Kling, I. A1 - Pauw, Brian Richard A1 - Agudo Jácome, Leonardo A1 - Archanjo, B. S. A1 - Simão, R. A. T1 - Development and characterization of starch film and the incorporation of silver nanoparticles N2 - Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties. T2 - Semana MetalMat & Painal PEMM 2020 CY - Online meeting DA - 23.11.2020 KW - Biofilm KW - Silver nanoparticle KW - Starch KW - Starch nanoparticle PY - 2020 SP - 1 EP - 2 AN - OPUS4-51940 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Suárez Ocano, Patricia A1 - Fries, S. G. A1 - Lopez-Galilea, I. A1 - Ruttert, B. A1 - Theissen, W. A1 - Agudo Jácome, Leonardo T1 - Effect of the heat treatment in the microstructure of a refractory chemically complex alloy N2 - A set of some unexpected and interesting microstructures has put the so-called complex concentrated alloys (CCAs) in the eye of the scientific community. The AlMo0.5NbTa0.5TiZr refractory (r)CCA, aimed at substituting Ni-base superalloys in gas turbine applications, belongs to this alloy family. After a two-stage heat treatment, this rCCA morphologically resembles the typical a two-phase microstructure of the latter. The objective of this work consists in determining the effect of the two stages of the heat treatment on the microstructure of the AlMo0.5NbTa0.5TiZr alloy to eventually improve it in terms of homogeneity and porosity. T2 - Third International Conference on High Entropy Materials (2020) CY - Berlin, Germany DA - 27.09.2020 KW - Annealing KW - Hot isostatic pressing KW - Refractory chemically complex alloy KW - Microstructure PY - 2020 AN - OPUS4-53386 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kling, I. C. S. A1 - Pauw, Brian Richard A1 - Agudo Jácome, Leonardo A1 - Archanjo, B. S. A1 - Simão, R. A. T1 - Development and characterization of starch film and the incorporation of silver nanoparticles N2 - Starch is one of the biopolymers being used for bioplastic synthesis. For production, starch can be combined with different plasticizers, starches from different plant sources and even with nanomaterials to improve or to add film properties. The challenge of adding these, e.g. in the form of silver nanoparticles (AgNp) is to determine the concentration so as to avoid impairing the properties of the film, agglomeration or altering the visual characteristics of the film. In this study, a starch film synthesis route and the incorporation of silver nanoparticles has been proposed in order not to alter the properties of the film while maintaining the transparency and a clear colour of the starch film. The results showed that the proposed synthesis route is promising, efficient, reproducible, fast and the film has good mechanical properties. T2 - Semana MetalMat & Painal PEMM 2020 CY - Online meeting DA - 23.11.2020 KW - Biofilm KW - Starch KW - Starch nanoparticle KW - Silver nanoparticle PY - 2020 AN - OPUS4-51828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Goedecke, Caroline A1 - Dittmann, Daniel A1 - Eisentraut, Paul A1 - Wiesner, Yosri A1 - Schartel, Bernhard A1 - Klack, Patrick A1 - Braun, Ulrike T1 - Evaluation of thermoanalytical methods equipped with evolved gas analysis for the detection of microplastic in environmental samples N2 - Microplastic particles are currently detected in almost all environmental compartments. The results of detection vary widely, as a multitude of very different methods are used with very different requirements for analytical validity. In this work four thermoanalytical methods are compared and their advantages and limitations are discussed. One of them is thermal extraction-desorption gas chromatography mass spectrometry (TED-GC/MS), an analysis method for microplastic detection that has become established in recent years. In addition, thermogravimetric analysis coupled with Fourier-transform infrared spectroscopy (TGA-FTIR) and mass spectrometry (TGA-MS) were applied, two methods that are less common in this field but are still used in other research areas. Finally, microscale combustion calorimeter (MCC) was applied, a method not yet used for microplastic detection. The presented results are taken from a recently published interlaboratory comparison test by Becker et al. (2020). Here a reference material consisting of suspended matter and specified added polymer masses was examined, and only the results of the recoveries were presented. In the present paper, however, the results for the individual polymers are discussed in detail and individual perspectives for all instruments are shown. It was found that TED-GC/MS is the most suitable method for samples with unknown matrix and unknown, variable kinds and contents of microplastic. TGA-FTIR is a robust method for samples with known matrix and with defined kinds of microplastic. TGA-MS may offer a solution for the detection of PVC particles in the future. MCC can be used as a very fast and simple screening method for the identification of a potential microplastic load of standard polymers in unknown samples. KW - Microplastic KW - TED-GC/MS KW - TGA-MS KW - TGA-FTIR KW - MCC KW - Thermal analysis PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-516687 DO - https://doi.org/10.1016/j.jaap.2020.104961 VL - 152 SP - 104961 PB - Elsevier B.V. AN - OPUS4-51668 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan-Scherb, Christiane A1 - Menneken, Martina A1 - Weber, Kathrin A1 - Agudo Jácome, Leonardo A1 - Nolze, Gert T1 - Elucidation of orientation relations between Fe-Cr alloys and corrosionproducts after high temperature SO2 corrosion N2 - The early stages of corrosion of Fe-Cr-model alloys (2 and 9 % Cr) were investigated after exposure at 650 °C in0.5 % SO2containing gas by electron backscattered diffraction (EBSD) and transmission electron microscopy(TEM). The impact of the grain orientation of the base alloy on the orientation relations of the corrosion productsis presented. After 2 min–5 min exposure the formation of a multi-layered corrosion zone was discovered. Aclear orientation relationship between ferrite and the (Fe,Cr)3O4 spinel could be demonstrated. The obtainedresults show the importance of the grain orientation on oxidation resistance. KW - Iron KW - TEM KW - SEM KW - High temperature corrosion PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508911 DO - https://doi.org/10.1016/j.corsci.2020.108809 VL - 174 SP - 1 EP - 11 PB - Elsevier AN - OPUS4-50891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Markwart, J. C. A1 - Battig, Alexander A1 - Urbaniak, T. A1 - Haag, K. A1 - Koschek, K. A1 - Schartel, Bernhard A1 - Wurm, F. R. T1 - Intrinsic flame retardant phosphonate-based vitrimers as a recyclable alternative for commodity polymers in composite materials N2 - Recycling of crosslinked fiber-reinforced polymers is difficult. Moreover, as they are often based on flammable resins, additional additives are needed. So-called “vitrimers” open the possibility of Recycling and reprocessing and repairing with dynamically crosslinked chemistries. To date, vitrimer-based composites still need flame retardant additives, such as organophosphates. An additive-free vitrimer composite has not been reported. Herein, we synthesized an intrinsic flame-retardant vitrimer, relying on vinylogous polyurethanes containing covalently installed phosphonates as flame-retardant units and prepared glassfiber-reinforced composites. We studied recycling and flame retardant properties and compared the data to phosphorus-free vitrimers and conventional epoxy resins (with and without additive flame retardant). Our phosphonate-based vitrimer proved in first tests, a flame retardant effect comparable to commercial flame retardant resins. The bending strength and bending modulus for the phosphorus-vitrimer glass fiber composites were comparable to glass fiber composites with permanently cross-linked epoxies. In summary, we were able to prove that the covalent installation of phosphonates into vitrimers allows the preparation of recyclable and intrinsic flame retardant composites that do not need flame retardant additives. We believe this concept can be expanded to other polymer networks and additives to generate recyclable and sustainable high-performance materials. KW - Vitrimer KW - Flame retardant KW - Recyclable KW - Organophosphonate KW - Polyurethane PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510889 DO - https://doi.org/10.1039/d0py00275e VL - 11 IS - 30 SP - 4933 EP - 4941 AN - OPUS4-51088 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Epping, Ruben A1 - Falkenhagen, Jana A1 - Panne, Ulrich A1 - Hiller, W. A1 - Gruendling, T. A1 - Staal, B. A1 - Lang, C. A1 - Lamprou, A. T1 - Simultaneous characterization of poly(acrylic acid) andpolysaccharide polymers and copolymers N2 - Copolymer products that result from grafting acrylic acid and other hydrophilicmonomers onto polysaccharides have recently gained significant interest in researchand industry. Originating from renewable sources, these biodegradable, low toxicity,and polar copolymer products exhibit potential to replace polymers from fossil sourcesin several applications and industries. The methods usually employed to character-ize these copolymers are, however, quite limited, especially for the measurement ofbulk properties. With more sophisticated applications, for example, in pharmaceu-tics requiring a more detailed analysis of the chemical structure, we describe a newapproach for this kind of complex polymers. Our approach utilizes chromatographyin combination with several detection methods to separate and characterize reactionproducts of the copolymerization of acrylic acid and chemically hydrolyzed starch.These samples consisted of a mixture of homopolymer poly (acrylic acid), homopoly-mer hydrolyzed starch, and – in a lower amount – the formed copolymers. Several chro-matographic methods exist that are capable of characterizing either poly (acrylic acid)or hydrolyzed starch. In contrast, our approach offers simultaneous characterization ofboth polymers. The combination of LC and UV/RI offered insight into the compositionand copolymer content of the samples. Size exclusion chromatography experimentsrevealed the molar mass distribution of homopolymers and copolymers. FTIR inves-tigations confirmed the formation of copolymers while ESI-MS gave more details onthe end groups of hydrolyzed starches and poly (acrylic acids). Evidence of copolymerstructures was obtained through NMR measurements. Finally, two-dimensional chro-matography led to the separation of the copolymers from both homopolymers as wellas the additional separation of sodium clusters. The methods described in this work area powerful toolset to characterize copolymerization products of hydrolyzed starch andpoly(acrylic acid). Together, our approach successfully correlates the physicochemicalproperties of such complex mixtures with their actual composition. KW - 2D chromatography KW - LC-MS KW - SEC KW - Renewable copolymers KW - Grafting PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-508873 DO - https://doi.org/10.1002/ansa.202000044 SP - 1 EP - 12 PB - Wiley-VCH Verlag-GmbH&Co. KGaA CY - Weinheim AN - OPUS4-50887 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, Sebastian A1 - Klack, Patrick A1 - Bahr, Horst A1 - Schartel, Bernhard T1 - Assessing the fire behavior of woods modified by N-methylol crosslinking, thermal treatment, and acetylation N2 - Wood products are often treated by different techniques to improve their longevity when used as building materials. Most of the time, the goal is to increase their resistance to weathering effects, deformations in material dimensions or biotic decomposition. These wood treatment techniques have a significant impact on pyrolysis and burning behavior. The general effects of three different common wood treatments on flame retardancy were investigated by comparing treated woods with their untreated counterparts and with other kinds of wood. While the acetylation of beech leads to a slightly increased fire hazard, the thermal treatment of wood and crosslinking of cellulose microfibrils dimethyloldihydroxy-ethyleneurea show a limited flame retarding effect. Switching to woods with a higher lignin content, and thus higher char yield, however, results in a more pronounced improvement in flame retardancy performance. This article delivers a comprehensive and balanced assessment of the general impact of different wood modifications on the fire behavior. Further, it is a valuable benchmark for assessing the flame retardancy effect of other wood modifications. KW - Acetylation KW - Cone claorimeter KW - DMDHEU KW - Heat of combustion KW - Thermal treatment KW - Wood modification PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-507397 DO - https://doi.org/10.1002/fam.2809 SN - 1099-1018 SN - 0308-0501 VL - 44 IS - 4 SP - 530 EP - 539 PB - Wiley Online Libary AN - OPUS4-50739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Höhne, Patrick A1 - Mieller, Björn A1 - Rabe, Torsten T1 - Advancing spray granulation by ultrasound atomization N2 - The influence of the atomization technique on the suitability of granules for dry pressing is the focus of the presented investigations. Therefore, destabilized alumina, zirconia, and zirconia toughened alumina (ZTA) slurries were spray dried and the obtained granules were used to fabricate green and finally sintered bodies for evaluation. Granules made in a laboratory spray dryer with a two-fluid nozzle served as a reference. An ultrasonic atomizer was integrated into the same spray dryer and the influence on the granule properties was evaluated. Untapped bulk density, granule size distribution, and flowability are among the evaluated granule-related properties as well as the granule yield which is used as an indicator of the process efficiency. Yield and flowability as most important granule properties are clearly improved when atomization is realized with ultrasound. The investigated sinter body properties include porosity, sinter body density, and biaxial strength and are as well positively affected by switching the atomization technique to ultrasound. Therefore, the Approach to improve the compressibility of granules by ultrasonic atomization, which leads to an improved microstructure, density, and strength of sintered bodies, has proven to be successful for single-component ceramics (alumina and zirconia) as well as for the multicomponent ceramic ZTA. KW - Alumina KW - Granules KW - Spray drying KW - Ultrasound KW - Zirconia KW - Zirconia-toughened alumina PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-510696 DO - https://doi.org/10.1111/ijac.13534 VL - 17 IS - 5 SP - 2212 EP - 2219 AN - OPUS4-51069 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Günther, Martin A1 - Lorenzetti, A. A1 - Schartel, Bernhard T1 - From Cells to Residues: Flame-Retarded Rigid Polyurethane Foams N2 - Rigid polyurethane foams (RPUFs) exhibit short times to ignition as well as rapid flame spread and are therefore considered to be hazardous materials. This paper focuses on the fire phenomena of RPUFs, which were investigated through a multimethodological approach. Water-blown polyurethane (PUR) foams without flame retardants (FRs) as well as waterblown PUR foams containing triethyl phosphate as a gas phase-active FR were examined. The aim of this study is to clarify the influence of the FR on the fire phenomena during combustion of the foams. Additionally, materials’ densitieswere varied to range from 30 to 100 kg/m3. Thermophysical properties were studied bymeans of thermogravimetry; fire behavior and flammability were investigated via cone calorimeter and limiting Oxygen index, respectively. During the cone calorimeter test, the temperature development inside the burning specimens was monitored with thermocouples, and cross sections of quenched specimens were examined visually, giving insight into the morphological changes during combustion. The present paper delivers a comprehensive study, illuminating phenomena occurring during foam combustion and the influence of a FR active in the gas phase. The superior fire performance of flameretarded PUR foams was found to be based on flame inhibition, and on increased char yield leading to a more effective protective layer. It was proven that in-depth absorption of radiation is a significant factor for estimation of time to ignition. Cross sections investigated with the electron scanning microscope exhibited a pyrolysis front with an intact foam structure underneath. The measurement of temperature development inside burning specimens implied a shift of burning behavior towards that of non-cellular materials with rising foam density. KW - Polyurethane KW - Rigid foams KW - Fire behavior PY - 2020 DO - https://doi.org/10.1080/00102202.2019.1634060 SN - 0010-2202 SN - 1563-521X VL - 192 IS - 12 SP - 2209 EP - 2237 PB - Taylor & Francis AN - OPUS4-51483 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Rabe, Sebastian A1 - Sanchez-Olivares, G. A1 - Pérez-Chávez, R. A1 - Schartel, Bernhard ED - Laoutid, F. T1 - Natural Keratin and Coconut Fibres from Industrial Wastes in Flame Retarded Thermoplastic Starch Biocomposites N2 - Natural keratin fibres derived from Mexican tannery waste and coconut fibres from coconut processing waste were used as fillers in commercially available, biodegradable thermoplastic starch-polyester blend to obtain sustainable biocomposites. The morphology, rheological and mechanical properties as well as pyrolysis, flammability and forced flaming combustion behaviour of those biocomposites were investigated. In order to open up new application areas for these Kinds of biocomposites, ammonium polyphosphate (APP) was added as a flame retardant. Extensive flammability and cone calorimeter studies revealed a good flame retardance effect with natural fibres alone and improved effectiveness with the addition of APP. In fact, it was shown that replacing 20 of 30 wt. % of APP with keratin fibres achieved the same effectiveness. In the case of coconut fibres, a synergistic effect led to an even lower heat release rate and total heat evolved due to reinforced char residue. This was confirmed via scanning electron microscopy of the char structure. All in all, these results constitute a good approach towards sustainable and biodegradable fibre reinforced biocomposites with improved flame retardant properties. KW - Biomaterials KW - Biodegradation KW - Calorimetry KW - Composites KW - Flame retardance PY - 2020 SN - 978-3-03928-350-7 SN - 978-3-03928-351-4 SP - 45 EP - 66 PB - MDPI AN - OPUS4-50738 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Famy, A. A1 - Agudo Jácome, Leonardo A1 - Schönhals, Andreas T1 - Effect of Silver Nanoparticles on the Dielectric Properties and the Homogeneity of Plasma Poly(acrylic acid) Thin Films N2 - For the first time, structure−electrochemical relationships of thin films of a plasma-polymerized acrylic acid/carbon dioxide AA/CO2 (75/25%) copolymer modified by implanted silver nanoparticles are discussed. The pulsed plasma polymerization of AA/CO2 was utilized and adjusted to obtain a maximal amount of COOH Groups forming an almost uncross-linked polymer structure. The prepared polymer layer is rinsed by a silver nitrate solution to impregnate Ag+ ions. This step is followed by its reduction of Ag+ with NaBH4 as a chemical route in comparison to the reduction by sunlight as an ecofriendly photoreduction method. The chemical composition and morphology of the topmost surface layer of the AA/CO2 polymer thin film were investigated by X-ray photoelectron spectroscopy and atomic force microscopy. Moreover, the molecular mobility, conductivity, and thermal stability of the polymer layer were analyzed using broadband dielectric spectroscopy. The dielectric properties of the AA/ CO2 polymer thin film were studied in the presence of Ag+ ions or Ag0. It was found that a cross-linked polymer layer with a smooth surface and high conductivity was obtained in the presence of Ag+/ Ag0. KW - Nanoparticles PY - 2020 DO - https://doi.org/10.1021/acs.jpcc.0c06712 SN - 1932-7447 VL - 124 IS - 41 SP - 22817 EP - 22826 PB - ACS AN - OPUS4-51468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Baumann, Maria A1 - Falkenhagen, Jana A1 - Weidner, Steffen A1 - Wold, C. A1 - Uliyanchenko, E. T1 - Characterization of copolymers of polycarbonate and polydimethylsiloxane by 2D chromatographic separation, MALDI-TOF mass spectrometry, and FTIR spectroscopy N2 - The structure and composition of polycarbonate polydimethylsiloxane copolymer (PC-co-PDMS) was investigated by applying various analytical approaches including chromatographic separation methods, spectrometric, and spectroscopic detection techniques. In particular, size exclusion chromatography (SEC) and liquid adsorption chromatography operating at different conditions (e.g. using gradient solvent systems) were used to achieve separations according to molar mass and functionality distribution. The coupling of both techniques resulted in fingerprint two-dimensional plots, which could be used to easily compare different copolymer batches. Matrix-assisted laser desorption/ionization-time-of-flight (MALDI-TOF) mass spectrometry was applied for structural investigations. The different ionization behavior of both comonomers, however, strongly limited the applicability of this technique. In contrast to that, Fourier-transform Infrared (FTIR) spectroscopy could be used to quantify the amount of PDMS in the copolymer at different points in the chromatogram. The resulting methodology was capable of distinguishing PC-co-PDMS copolymer from PC homopolymer chains present in the material. KW - FTIR KW - Liquid chromatography KW - Mass spectrometry KW - Gradient elution KW - Polycarbonate-co-dimethylsiloxane copolymer PY - 2020 DO - https://doi.org/10.1080/1023666X.2020.1820170 VL - 25 IS - 7 SP - 1 EP - 12 PB - Taylor & Francis AN - OPUS4-51369 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -