TY - JOUR A1 - Peplinski, Burkhard A1 - Adamczyk, Burkart A1 - Formanek, P. A1 - Meyer, Christian A1 - Krüger, O. A1 - Scharf, Holger A1 - Reinsch, Stefan A1 - Ostermann, Markus A1 - Nofz, Marianne A1 - Jäger, Christian A1 - Adam, Christian A1 - Emmerling, Franziska T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4 chemically stabilized at room temperature: synthesis, physical characterization, and X-ray powder diffraction data N2 - This paper reports the first successful synthesis and the structural characterization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 that is chemically stabilized down to room temperature and free of crystalline impurity phases. Several batches of the title compound were synthesized and thoroughly characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy, selected area electron diffraction, energy dispersive X-ray spectroscopy mapping in SEM, solid-state 31P nuclear magnetic resonance (31P-NMR) spectroscopy including the TRAPDOR method, differential thermal analysis (DTA), gas-sorption methods, optical Emission spectroscopy, X-ray fluorescence spectroscopy, and ion chromatography. Parameters that are critical for the synthesis were identified and optimized. The synthesis procedure yields reproducible results and is well documented. A high-quality XRD pattern of the title compound is presented, which was collected with monochromatic copper radiation at room temperature in a wide 2θ range of 5°–100°. KW - Stabilization of high-temperature phase at RT KW - Nanochrystalline AlPO4 KW - Beta-christobalite structure type KW - High-cristobalite form KW - Aluminium phosphate PY - 2017 DO - https://doi.org/10.1017/S0885715617000537 SN - 1945-7413 SN - 0885-7156 VL - 32 IS - S1 SP - S193 EP - S200 PB - JCPDS-ICDD CY - Cambridge AN - OPUS4-42235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vogel, Christian A1 - Hermann, P. A1 - Kästner, B. A1 - Adamczyk, Burkart A1 - Hoehl, A. A1 - Ulm, G. A1 - Adam, Christian T1 - Air and chlorine gas corrosion of different silicon carbides analyzed by nano-Fourier-transform infrared (nano-FTIR) spectroscopy N2 - The present study shows the potential of high-resolution imaging and nano-Fourier-transform infrared (nano-FTIR) spectroscopy for corrosion science. The protective oxidation layers of different chlorine-gas treated silicon carbides (SiCs) were characterized with these techniques. A nitrified SiC showed the highest resistant strength against chlorine corrosion at 1000 °C compared to the other SiCs. Nano-FTIR spectroscopy with a lateral resolution below 40 nm detected differences in the crystallinity of the bulk-SiC and in the transitional region to the protective layer. Furthermore, high-resolution imaging provides deep insight in the interfacial layer between bulk-SiC and the protective oxidation layer on sub-micrometer scale. KW - Nano-Fourier-transform infrared spectroscopy KW - Scattering-type scanning near-field optical microscopy (s-SNOM) KW - Synchrotron radiation KW - Corrosion KW - Silicon carbide KW - Chlorine PY - 2018 DO - https://doi.org/10.1016/j.corsci.2017.12.002 SN - 0010-938X VL - 131 SP - 324 EP - 329 PB - Elsevier AN - OPUS4-43648 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Reuther, H. A1 - Vogel, Christian A1 - Adamczyk, Burkart A1 - Menzel, Michael A1 - Emmerling, Franziska A1 - Simon, Franz-Georg T1 - First identification of the tridymite form of AlPO4 in municipal sewage sludge ash N2 - Sewage sludge and sewage sludge ashes (SSA) are produced in huge amounts at municipal waste water treatment plants (WWTP) all around the world and have become an issue for many urbanized areas. To deal with this unceasing mass flow in an ecologically and economically responsible way a comprehensive chemical and structural characterization of all types of SSA is needed. X-ray powder diffraction (XRD) is one of the most promising analytical methods for this task. Although, there has been ample chemical evidence showing that many SSA contain aluminium phosphate as a major component up to now no aluminium phosphate or aluminium-rich mixed phosphate phase has been reported to be identified by XRD in a SSA produced at a mono-incineration facility. The outcome of the present com-bined XRD and Mossbauer spectroscopy investigation provides comprehensive evidence closing this gap for the first time. KW - Aluminium phosphate KW - AlPO4 KW - Tridymite KW - Sewage sludge ash KW - Incinerator KW - Ash PY - 2011 DO - https://doi.org/10.1524/zkpr.2011.0067 SN - 0044-2968 VL - 1 SP - 443 EP - 448 PB - Oldenbourg CY - München AN - OPUS4-24297 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schraut, Katharina A1 - Adamczyk, Burkart A1 - Adam, Christian A1 - Stephan, Dietmar A1 - Meng, Birgit A1 - Simon, Sebastian A1 - von Werder, Julia A1 - Hirsch, Tamino A1 - Manninger, Tanja T1 - Effect of gypsum on the hydration of fused cement clinker from basic oxygen furnace slag N2 - Fused cement clinker can be produced from molten basic oxygen furnace slag (BOFS) by way of a reductive thermochemical treatment. During the thermochemical treatment, oxidic iron is reduced to metallic iron and separated. The resulting low-iron slag has a chemical and mineralogical composition similar to ordinary Portland cement (OPC) clinker. In this study, the hydraulic reactivity of the fused clinker from BOFS with and without gypsum was investigated using isothermal calorimetry, differential scanning calorimetry, in situ X-ray diffraction and powder X-ray diffraction. Furthermore, a synthetic fused clinker without foreign ions and fused clinker produced by a mixture of both materials was studied. The hydraulic reaction of the fused clinker from BOFS was considerably slower than that of OPC. However, the reaction can be accelerated by adding gypsum as a sulfate carrier. Furthermore, the results showed an increased reaction rate with decreasing content of foreign ions such as Fe, P or Mn. KW - General Materials Science KW - Building and Construction PY - 2024 DO - https://doi.org/10.1680/jadcr.23.00070 SN - 0951-7197 SP - 1 EP - 19 PB - Telford AN - OPUS4-59391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schraut, Katharina A1 - Adamczyk, Burkart A1 - Simon, Sebastian A1 - von Werder, Julia A1 - Meng, Birgit A1 - Stephan, D. A. A1 - Adam, Christian T1 - Zementklinker durch Nachbehandlung von Stahlwerksschlacken N2 - Die Klinkerphasenbildung durch Sinterung in Drehrohröfen bei der Herstellung von Portlandzementklinker (PZK) ist gründlich erforscht und optimiert. Im Hinblick auf mögliche ökonomische und ökologische Vorteile befassen sich aktuelle Forschungsvorhaben darüber hinaus mit der Herstellung von Klinkermineralen aus Stahlwerksschlacken, die eine vergleichbare chemische Zusammensetzung aufweisen. Neuste Untersuchungen zeigen, dass nach der reduzierenden Behandlung schmelzflüssiger Linz-Donawitz-(LD)-Schlacken und Abscheidung des gebildeten metallischen Eisens eine mineralische Schlacke entsteht, die unabhängig von ihren Abkühlbedingungen ca. 50–60 Gew.% des wichtigsten Klinkerminerals Alit (C3S) enthält und eine hohe hydraulische Reaktivität aufweist. Die Stabilität des Alits auch nach langsamer Abkühlung deutet auf eine Stabilisierung des Minerals durch Nebenelemente aus den LD-Schlacken hin. Ein sinkender Anteil an LD-Schlacke durch Zusatz synthetischer Schlackemischung, die sich hinsichtlich ihrer Hauptkomponenten wie eine ausreduzierte LD-Schlacke zusammensetzt, führt zu einem Rückgang des Alitgehaltes und dem Zerfall der Schlacke beim Erstarren. T2 - 5. Schlacken-Symposium CY - Meitingen, Germany DA - 25.10.2018 KW - LD-Schlacke KW - Zement KW - Tricalciumsilikat PY - 2018 SP - 219 EP - 229 PB - Max Aicher Unternehmensgruppe AN - OPUS4-46412 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Taube, Mareike Carolin A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Schulenburg, F. A1 - Bartmann, U. A1 - Beckmann, T. A1 - Michalik, K. A1 - Reuter, M. A1 - Stelter, M. T1 - Optimisation of a Pyrometallurgical Niobium and Tantalum Recyling Process with on-line-LIBS N2 - Tantalum and niobium are essential for the development of electronics towards a more and more compact design, but without reducing their performance today. Especially in smart phones and tablets, tantalum and niobium capacitors with high charge densities have already become almost indispensable. However, tantalum as a critical raw material is still a problem for the sustainable production of electronics. Due to this fact, the existence of efficient recycling processes especially in Europe is becoming even more important nowadays. The Bundesanstalt für Materialforschung und -prüfung (BAM) is currently working on the optimisation of an existing pyrometallurgical tantalum recycling process. Optimisation of this industrial process is carried out in a small-scale electric arc furnace (480 kVA, capacity approx. 150 kg/h) at BAM using a new and innovative equipment for on-line analysis of high temperature processes. The aim of this project is to identify the best timing for an optimum slag tapping, when the slag is lower than minimum targeted tantalum concentration. Hence, LIBS (Laser induced breakdown spectroscopy) is used to identify the chemical composition of the slag layer and during slag tapping. The on-line-LIBS prototype of BAM enables an in-situ measurement of the element distribution in the melt after calibration on the slag system. First results of this joint research project will be presented including LIBS-measurements and thermodynamic and kinetic aspects of the process. T2 - European Mineral Processing & Recycling Congress (EMPRC 2018) CY - Essen, Germany DA - 25.06.2018 KW - Laser-induced breakdown spectroscopy KW - On-line analysis KW - Tantalum KW - Niobium KW - Pyrometallurgy PY - 2018 SN - 978-3-940276-84-1 SP - 347 EP - 362 PB - GDMB Verlag GmbH CY - Clausthal-Zellerfeld AN - OPUS4-47040 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Taube, Mareike Carolin A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Beckmann, T. A1 - Reuter, M. A1 - Stelter, M. T1 - Influence of carbon feeding on a pyrometallurgical tantalum and niobium recycling process and the formation of carbides N2 - An existing pyrometallurgical process for tantalum and niobium recovery, mainly from low grade pyrometallurgical residues, was investigated. Series of melting experiments were carried out in a pilot-scale electric arc furnace to study how the amount, the grain size and the way of feeding affect the activity of carbon as a reducing agent. During the pyrometallurgical treatment refractory metals such as tantalum and niobium are reduced to their carbide form and enriched in the molten iron-based metal phase. The cooled down slag and metal phase were analysed to investigate thermodynamic and kinetic conditions of the carbide formation. FACT Sage simulations were also used to investigate the material system in state of thermodynamic equilibrium. Results show that mass transfer and kinetics may play an important role if compared to equilibrium analyses using FACT Sage. T2 - Euopean Metallurgical Conference (EMC) 2019 CY - Düsseldorf, Germany DA - 23.06.2019 KW - Pyrometallurgy KW - Tantalum KW - Carbide formation KW - Reduction process KW - Carbon feeding PY - 2019 SN - 978-3-940276-87-2 VL - 1 SP - 371 EP - 386 PB - GDMB Verlag GmbH CY - Clausthal-Zellerfeld AN - OPUS4-48363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Taube, Mareike Carolin A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Beckmann, T. A1 - Reuter, M. A1 - Stelter, M. ED - Thiel, S. ED - Thomé-Kozmiensky, E. ED - Pretz, T. ED - Senk, D. G. ED - Wotruba, H. T1 - Tantal-Rückgewinnung aus Zinnschlacken und weiteren Reststoffen N2 - Since the recycling of tantalum bearing post-consumer waste is practically not existent, metallurgical residues are the most important feed for the tantalum recycling. Most tin ores naturally contain significant quantities of refractory metals. During the smelting process in primary tin production these elements are enriched in the slag phase. This slag is a highly valuable raw material for tantalum production due to its considerable concentration of tantalum and its functioning as an additional slag former in further pyrometallurgical treatment. In this paper the first process stage of an existing pyrometallurgical process for tantalum recovery, mainly from low grade pyrometallurgical residues, is discussed. Smelting trials were carried out in a pilot-scale electric arc furnace to analyse the effect of feeding on the activity of carbon as a reducing agent. Therefore, blowing petroleum coke through an iron lance and the manual adding of coke into the melting bath were tested. During the pyrometallurgical treatment elements with a high affinity to carbon were reduced to their carbide form and enriched in the molten iron-based metal phase. The objective of the process was to reduce the oxidic tantalum completely and to enrich it into the metal phase. Furthermore, the transfer of unwanted elements such as titanium into the metal phase was aimed to be avoided. Spoon test specimens were taken from the liquid mineral melt to follow the evolution of the reduction process. The cooled down solidified melting bath was investigated by using the XRD and EDX method to characterise the slag system and to identify relevant mineral phases. T2 - Berliner Konferenz Mineralische Nebenprodukte und Abfälle CY - Berlin, Germany DA - 13.05.2019 KW - Zinnschlacke KW - Tantal KW - Recycling KW - Pyrometallurgie KW - Lichtbogenofen PY - 2019 SN - 978-3-944310-47-3 VL - 6 SP - 378 EP - 393 PB - Thomé-Kozmiensky Verlag GmbH CY - Neuruppin AN - OPUS4-48357 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schneider, Joachim A1 - Adamczyk, Burkart A1 - Ebert, D. A1 - Ehrenberg, A. A1 - Schraut, Katharina A1 - Gerlach, J. A1 - Wendt, K. A1 - Algermissen, D. A1 - Adam, Christian ED - Rogge, Andreas ED - Meng, Birgit T1 - Erzeugung von Bindemitteln aus Stahlwerksschlacken N2 - Die geplante Transformation der Stahlindustrie innerhalb der nächsten 20 Jahre hat aufgrund des mit ihr verbundenen Auslaufens der Hüttensanderzeugung Konsequenzen für die Zementindustrie, deren Abmilderung Gegenstand der Forschungsprojekte SlagCEM und DRI-EOS ist. Ersteres untersucht die Rückgewinnung von Eisen aus LD-Konverter-Schlacke bei gleichzeitiger Herstellung eines mineralischen Produktes mit zementä- ren Eigenschaften. Zweiteres befasst sich mit der Generierung eines Hüttensandersatzes aus Lichtbogen- ofenschlacke mit Rückgewinnung von Schwermetallen sowie deren Umwelteffekt bei Verbleib in der Schlacke. T2 - 11. Jahrestagung des DAfStb mit 63. Forschungskolloquium der BAM Green Intelligent Building CY - Berlin, Germany DA - 16.10.2024 KW - Bindemittel KW - Stahlwerksschlacke PY - 2024 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-613127 SN - 978-3-9818564-7-7 SP - 78 EP - 89 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-61312 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Taube, Mareike Carolin A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Beckmann, T. A1 - Reuter, M. A1 - Stelter, M. ED - Reiser, B. T1 - Recycling von metallurgischen Rückständen - Schmelzversuche zeigen, wie die Tantalrückgewinnung aus Zinnschlacken und weiteren Reststoffen optimiert werden kann N2 - Since the recycling of tantalum bearing post-consumer waste is practically not existent, metallurgical residues are the most important feed for the tantalum recycling. Most tin ores naturally contain significant quantities of refractory metals. During the smelting process in primary tin production these elements are enriched in the slag phase. This slag is a highly valuable raw material for tantalum production due to its considerable concentration of tantalum and its functioning as an additional slag former in further pyrometallurgical treatment. In this paper the first process stage of an existing pyrometallurgical process for tantalum recovery, mainly from low grade pyrometallurgical residues, is discussed. Smelting trials were carried out in a pilot-scale electric arc furnace to analyse the effect of feeding on the activity of carbon as a reducing agent. Therefore, blowing petroleum coke through an iron lance and the manual adding of coke into the melting bath were tested. During the pyrometallurgical treatment elements with a high affinity to carbon were reduced to their carbide form and enriched in the molten iron-based metal phase. The objective of the process was to reduce the oxidic tantalum completely and to enrich it into the metal phase. Furthermore, the transfer of unwanted elements such as titanium into the metal phase was aimed to be avoided. Spoon test specimens were taken from the liquid mineral melt to follow the evolution of the reduction process. The cooled down solidified melting bath was investigated by using the XRD and EDX method to characterise the slag system and to identify relevant mineral phases. N2 - Da das Recycling von tantalhaltigen Post-Consumer-Abfällen praktisch nicht existiert, stellen metallurgische Reststoffe eine äußerst wichtige Rohstoffquelle für das Tantalrecycling dar. Die meisten Zinnerze enthalten von Natur aus erhebliche Mengen an Refraktärmetallen. Diese Elemente werden in den Schlacken der pyrometallurgischen Primärzinngewinnung angereichert. Aufgrund ihrer vergleichsweise hohen Wertstoffkonzentration und ihrer Funktion als zusätzlicher Schlackenbildner stellen diese Schlacken einen wertvollen Rohstoff für die Verhüttung tantalhaltiger Reststoffe dar. In der vorliegenden Arbeit wird ein existierendes Verfahren zur Tantalrückgewinnung diskutiert, dem hauptsächlich pyrometallurgische Rückstände geringer Wertstoffkonzentration als Einsatzstoff dienen. Mit Hilfe des Verfahrens sollte dasoxidisch vorliegende Tantal vollständig reduziert und in der Metallphase angereichert werden. Weiterhin sollte vermieden werden, dass unerwünschte Elemente wie Titan in die Metallphase überführt werden. Ziel der Untersuchung war es, die ablaufenden Reduktionsprozesse besser zu verstehen, um so Ansätze für die Prozessoptimierung identifizieren zu können. KW - Lichtbogenofen KW - Pyrometallurgie KW - Recycling KW - Tantal KW - Zinnschlacke PY - 2020 SN - 0934-3482 VL - 33 SP - 10 EP - 17 PB - Rhombos-Verlag CY - Berlin AN - OPUS4-50656 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -