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- Aluminium phosphate (3)
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- Nano-Fourier-transform infrared spectroscopy (1)
- Nanochrystalline AlPO4 (1)
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Organisationseinheit der BAM
Slags from the production of high-alloyed steel contain both chemically bound chromium (mainly as Cr2O3) in the mineral fraction and elemental chromium in the metallic remainders. Thermochemical post treatment of the slag in an electric arc furnace under reducing conditions enables the nearly complete recovery of the total amount of chromium in form of a metallic alloy. The best results were achieved by resistance melting (submerged electrodes) with addition of a reducing agent into the melt. The efficiencies of the reducing agents carbon, aluminium, silicon (as ferrosilicon) and silicon carbide were investigated and compared. As aluminium is the strongest reducing agent, it is less selective and reduces much more SiO2 than Cr2O3. While SiC shows only low reactivity because of its high thermal resistance, carbon and silicon had the highest reducing potentials: More than 97% of the chemically bound chromium can be recovered by application of these reducing agents. Due to the high temperature required for the reduction of the chromium compounds, the reduction of SiO2 as an undesired side reaction cannot be avoided. However, compared with mechanical procedures that are limited to the recovery of the metallic remainders, the total chromium recovery can be significantly increased by the described reductive melting procedure.
For the first time evidence is provided that a nanocrystalline and stacking-disordered, chemically stabilized β-cristobalite form of AlPO4 occurs in a sewage sludge ash (SSA). This proof is based on a combined X-ray powder diffraction and X-ray fluorescence investigation of an SSA produced at a large-scale fluidized bed incineration facility serving a catching area with a population of 2 million. The structural and chemical characterization was carried out on 'as received' SSA samples as well as on solid residues remaining after leaching this SSA in sodium hydroxide solution. Thus, it was ascertained that the observed nanocrystalline and stacking-disordered cristobalite-like component belongs to the aluminum phosphate component of this SSA, rather than to its silicon dioxide component. In addition, a direct proof is presented that the chemically stabilized β-cristobalite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850°C), typical for fluidized bed incinerators.
Gegenstand dieser Arbeit ist die Untersuchung eines bestehenden pyrometallurgischen Prozesses zur Rückgewinnung von Tantal und Niob aus metallurgischen Reststoffen mit vorwiegend niedriger Wertstoffkonzentration.
Zur näheren Erforschung der im vorliegenden Stoffsystem ablaufenden Reduktionsprozesse wurden in einem Elektrolichtbogenofen Schmelzversuche im Pilotmaßstab durchgeführt. Als Reduktionsmittel diente Koks, welcher mithilfe einer Argon-gespülten Eisenlanze in die flüssige mineralische Schmelze eingebracht wurde. Während der Reduktionsbehandlung werden Refraktärmetalle wie Tantal und Niob in ihre Carbide überführt und anschließend in der erschmolzenen eisenbasierten Metallphase am Boden des Reaktors angereichert. Neben Tantal und Niob gelangt auch ein Teil des im Einsatzmaterial enthaltenen Titans als unerwünschtes Begleitelement in die Metallphase.
Sein Großteil verbleibt jedoch als Oxid in der Schlacke und wird dort hauptsächlich im Mineral Perowskit (CaTiO3) gebunden. Die erstarrten Schlackeproben wurden mit verschiedenen Methoden wie Röntgenfluoreszensanalyse, Röntgenbeugung und Rasterelektronenmikroskopie mit gekoppelter energiedispersiver Röntgenanalyse untersucht, um die Bildung tantalhaltiger Mineralphasen zu verschiedenen Stadien des Reduktionsprozesses zu verfolgen.
Die hier gewonnenen Erkenntnisse zeigen, dass weniger die durch das Einblasen von Koks verursachte Reduktionsreaktion, sondern das Absinken der tantalreichen Eisentröpfchen in der flüssigen mineralischen Schmelze, gefolgt von ihrer Anreicherung in die Metallphase, für die Kinetik ausschlaggebend ist.
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.
Based on recently published research on leaching control mechanisms in electric arc furnace (EAF) slags, it is assumed that a FeO/SiO2 ratio of around one leads to low leached V and Cr concentrations. This ratio influences the mineral phase composition of the slag toward higher amounts of spinel and a lower solubility of calcium silicate phases by suppressing the formation of magnesiowuestite and highly soluble calcium silicate phases. To evaluate this hypothesis, laboratory and scaled up tests in an EAF pilot plant were performed on slag samples characterized by elevated V and Cr leaching and a high FeO/SiO2 ratio. Prior to the melting experiments, the optimum FeO/SiO2 ratio was calculated via FactSageTM. In the melting experiments, the ratio was adjusted by adding quartz sand, which also decreased the basicity (CaO/SiO2) of the slag. As a reference, remelting experiments without quartz sand addition were conducted and additionally, the influence of the cooling rate of the slag was examined. The remelted (without quartz sand) and the remelted modified slags (with quartz sand) were analyzed chemically and mineralogically and the leaching behavior was investigated. The modification of the slags yielded a minimized release of V and Cr, supporting the hypothesis that the FeO/SiO2 ratio influences the mineralogy and the leaching behavior.
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.
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°.
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.
The recycling of refractory materials in the chemical, metallurgical and glass industry has only had minor relevance until now because of the high performance required from these materials (stability against corrosion, inert when coming into contact with the glass melt, etc.). Refractory lifetimes are limited because of corrosion at higher temperatures. The best furnace lifetimes has been achieved with chromium oxide and chromium oxide corund refractories. Waste from the production and use of refractory material is generated in three main forms: as residues from cutting and grinding, as refractories which have limited or no contact with glass melts, and as refractories with infiltration of sublimation residues or condensates. The waste material is classified as hazardous waste due to its chromium content. In this study, arc furnace technology was used for thermal treatment of the waste materials to enable recycling of refractory materials. (author abst.)