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- ItemA Highly Active Cobalt Catalyst for the General and Selective Hydrogenation of Aromatic Heterocycles(Weinheim : Wiley-VCH, 2023) Bauer, Christof; Müller, Felix; Keskin, Sercan; Zobel, Mirijam; Kempe, RhettNanostructured earth abundant metal catalysts that mediate important chemical reactions with high efficiency and selectivity are of great interest. This study introduces a synthesis protocol for nanostructured earth abundant metal catalysts. Three components, an inexpensive metal precursor, an easy to synthesize N/C precursor, and a porous support material undergo pyrolysis to give the catalyst material in a simple, single synthesis step. By applying this catalyst synthesis, a highly active cobalt catalyst for the general and selective hydrogenation of aromatic heterocycles could be generated. The reaction is important with regard to organic synthesis and hydrogen storage. The mild reaction conditions observed for quinolines permit the selective hydrogenation of numerous classes of N-, O- and S-heterocyclic compounds such as: quinoxalines, pyridines, pyrroles, indoles, isoquinoline, aciridine amine, phenanthroline, benzofuranes, and benzothiophenes.
- ItemSelective Pb2+ removal and electrochemical regeneration of fresh and recycled FeOOH([Erscheinungsort nicht ermittelbar] : Tsinghua Press, 2023) Wang, Lei; Deligniere, Lexane; Husmann, Samantha; Leiner, Regina; Bahr, Carsten; Zhang, Shengjie; Dun, Chaochao; Montemore, Matthew M.; Gallei, Markus; Urban, Jeffrey J.; Kim, Choonsoo; Presser, VolkerHeavy metal pollution is a key environmental problem. Selectively extracting heavy metals could accomplish water purification and resource recycling simultaneously. Adsorption is a promising approach with a facile process, adaptability for the broad concentration of feed water, and high selectivity. However, the adsorption method faces challenges in synthesizing high-performance sorbents and regenerating adsorbents effectively. FeOOH is an environmentally friendly sorbent with low-cost production on a large scale. Nevertheless, the selectivity behavior and regeneration of FeOOH are seldom studied. Therefore, we investigated the selectivity of FeOOH in a mixed solution of Co2+, Ni2+, and Pb2+ and proposed to enhance the capacity of FeOOH and regenerate it by using external charges. Without charge, the FeOOH electrode shows a Pb2+ uptake capacity of 20 mg/g. After applying a voltage of −0.2/+0.8 V, the uptake capacity increases to a maximum of 42 mg/g and the desorption ratio is 70%–80%. In 35 cycles, FeOOH shows a superior selectivity towards Pb2+ compared with Co2+ and Ni2+, with a purity of 97% ± 3% in the extracts. The high selectivity is attributed to the lower activation energy for Pb2+ sorption. The capacity retentions at the 5th and the 35th cycles are ca. 80% and ca. 50%, respectively, comparable to the chemical regeneration method. With industrially exhausted granular ferric hydroxide as the electrode material, the system exhibits a Pb2+ uptake capacity of 37.4 mg/g with high selectivity. Our work demonstrates the feasibility of regenerating FeOOH by charge and provides a new approach for recycling and upcycling FeOOH sorbent. [Figure not available: see fulltext.]
- ItemGrowth of titania and tin oxide from Ti2SnC via rapid thermal oxidation in air for lithium-ion battery application(Oxford [u.a.] : Wiley-Blackwell, 2023) Jolly, Shae; Husmann, Samantha; Presser, Volker; Naguib, MichaelHerein, we report the synthesis of TiO2–SnO2–C/carbide hybrid electrode materials for Li-ion batteries (LIBs) via two different methods of controlled oxidation of layered Ti2SnC. The material was partially oxidized in an open-air furnace (OAF) or using a rapid thermal annealing (RTA) approach to obtain the desired TiO2–SnO2–C/carbide hybrid material; the carbide phase encompassed both residual Ti2SnC and TiC as a reaction product. We tested the oxidized materials as an anode in a half cell to investigate their electrochemical performance in LIBs. Analysis of the various oxidation conditions indicated the highest initial lithiation capacity of 838 mAh/g at 100 mA/g for the sample oxidized in the OAF at 700°C for 1 h. Still, the delithiation capacity dropped to 427 mAh/g and faded over cycling. Long-term cycling demonstrated that the RTA sample treated at 800°C for 30 s was the most efficient, as it demonstrated a reversible capacity of around 270 mAh/g after 150 cycles, as well as a specific capacity of about 150 mAh/g under high cycling rate (2000 mA/g). Given the materials’ promising performance, this processing method could likely be applied to many other members of the MAX family, with a wide range of energy storage applications.
- Itemstress generation modulus as a counterpart of the stress relaxation modulus(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 1995) Brückner, Rolf; Hessenkemper, Heiko; Habeck, Andreas; Yue, YuanzhengIn order to measure the time dependence of the stress relaxation modulus, E, a stress-strain deformation has to precede which induces a stress within the viscoelastic sample from which the sample relaxes. The generation of stress is characterized by a strain rate-dependent and relaxation rate-dependent portion which exhibits a maximum value, E_max, which is called "stress generation modulus". E_max was called the "maximum stress relaxation modulus" in earlier papers. Meanwhile, however, it turned out that a better verbal distinction should be made in future by the new term "stress generation modulus" because E_max is about one order of magnitude larger than E.
- ItemZerstörungskennlinien für Verbundsicherheitsglasscheiben(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2001) Mayrhofer, Christoph; Kranzer, CarolineFür die Bewertung des Tragverhaltens von Bauteilen bei Explosionsereignissen sind sogenannte „Druck-Impuls-Diagramme" erforderlich. Diese geben in Abhängigkeit vom Druck und dem Impuls der Belastung an, für welche Wertepaare Zerstörung eintritt und welchen Belastungswerten das betrachtete Bauteil standhält. Derartige Zerstörungskennlinien sind am Fraunhofer EMI für eine Vielzahl von Werkstoffen entwickelt worden. Den Zerstörungskennlinien liegt das Rechenmodell des Ein-Massen-Schwingers zugrunde. Voraussetzungen für seine Anwendbarkeit sind Biegetragmechanismen, Bruch- bzw. Zerstörungskriterien (z.B. Grenzdurchbiegung) und die Kenntnis des statischen Last-Verformungsverhaltens. Untersuchungen ergaben, daß Verbundsicherheitsglasscheiben die Voraussetzungen für die Erstellung von Zerstörungskennlinien erfüllen. Es wird eine Näherungsmethode zur Erfassung des statischen Tragverformungsverhaltens unter Berücksichtigung von Membranspannungszuständen dargestellt. Am Beispiel anderer Werkstoffe wird die prinzipielle Vorgehensweise erläutert, da für Verbundsicherheitsscheiben bisher noch keine Bruchkriterien zur Verfügung stehen.
- ItemCollaborative study into the analysis of total selenium and selenium valence states in glass - a general method by hydride generation atomic absorption spectrometry and photometry : Report of the International Commission on Glass (ICG) Technical Committee 2 "Chemical Durability and Analysis"(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2000) Guadagnino, Emanuel; Çorumluoğlu, OrhanWhilst the determination of total selenium in glass is of great relevance to environmental purposes, the measurement of the oxidation states of selenium which may arise under different redox conditions may contribute to clarify the mechanisms of colour formation. In the proposed method, the determination of total selenium is carried out by hydride generation atomic absorption spectrometry (HGAAS) on three different glasses covering the range of selenium content between 10 and 130 mg/kg of glass. To prevent losses during the decomposition step, selenium is converted into a nonvolatile form as selenate (Se6+). When the sample is decomposed, the HCl Solution (c(HC1) = 10 mol/l) is made and selenium is pre-reduced to Se4+ by heating for 2 h at 80 °C. The determination of selenium oxidation states requires a stepwise approach. The measurement of Se0 is based on its insolubility in HF. After the sample is decomposed, Se0 is filtered off, dissolved from the filter with a HBr-Br2 mixture and finally measured by HGAAS. Se4+ and Se6+ are recovered in the filtrate of the same sample and determined together after conversion of Se4+ into Se6+. Se4+ is determined in the same filtrate by photometry with o-phenylenediamine (OPDA).
- ItemAdvanced oxygen burner for the glass industry(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 1997) Legiret, Thierry; Philippe, Louis; Tsiava, Remi; Marié, Bruno[no abstract available]
- ItemStudy of surface changes on industrial glasses with AFM, FE-SEM, EDX, SNMS and LM : Part 1. Glass skin and corrosion(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2004) Wang, Chun; Häfner, Wolfgang; Krausch, Georg; Rädlein, Edda; Tratzky, Stephan; Schramm, Manfred; Martinek, Klaus-PeterBy combining different analytieal techniques, including modern high resolution imaging tools such as field emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM), new phenomena in the surface, near surface and bulk structure of various industrial glasses (without any cleaning process) have been diseovered. Investigations of soda-lime-silica container glass and lead silicate glass tubings exposed to atmospheric and to dried air are presented. The results of the first part of this paper can be explained with an SiO2 rich skin on the glass, which can protect the glass against the attack of external media. If the skin was mechanically injured, inhomogeneous corrosion products on pm scale grew around the injured site after exposure to humid air for times between days up to one year. Microchannels were formed through the injured site due to restricted ion exchange, followed by a local increase of the pH value and consequently the dissolution of the glass network. Finally some stress in the glass, yielded during manufacture, can be partially released and the cutting behaviour is improved. Faster cooling results in a thinner skin and the ions in the glass are able to migrate to the surface more easily when surrounded by some reactive media. Slower cooling results in thicker skin and wax-like droplets instead of erystallites are formed on the surface at a later stage in humid air. The wax-like droplets can etch the glass skin locally, followed by the growth of inhomogeneous corrosion products similar to the injury induced corrosion. If the fresh glass surface was hot-end treated, the quality of the adjacent coating layer depended strongly on the thickness of the skin.
- ItemThermodynamic calculations of chemical solubilities of gases in oxide melts and glasses(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 1999) Pelton, Arthur D.The Reddy-Blander thermodynamic model for calculating sulfide solubilities in oxide melts and glasses has been modified and extended to predict a priori solubilities of sulfide, sulfate, phosphate, carbonate and halides in multicomponent oxide melts and glasses, from a knowledge of the thermodynamic activities of the basic component oxides (SiO₂, Na₂O, K₂O, CaO, etc.), in most cases with no adjustable parameters. Agreement with measured solubilities is within or nearly within experimental uncertainties over wide ranges of composition in two-, three-, four- and five-component melts and glasses. Particularly good agreement is obtained for the dissolution of sulfur, SO₂ and SO₃ as sulfate. The oxide activities used in the computations are calculated from a database of model parameters obtained by optimizing thermodynamic and phase equilibrium data for oxide Systems. Sulfide, sulfate, phosphate, carbonate and halides as solutes have now been included in this database. Software for Gibbs energy minimization with automatic access to this and other databases permits the calculation of solubilides in multicomponent oxide melts and glasses in equilibrium with other phases such as gases, molten salts, solids and metals, and can be useful to model evaporation processes and bubble formation.
- ItemInfluence of modifier cations on the radiation-induced effects of metaphosphate glasses(Offenbach : Verlag der Deutschen Glastechnischen Gesellschaft, 2003) Ebeling, Polina; Ehrt, Doris; Friedrich, ManfredThe influence of different modifying cations on the radiation-induced defect generation in metaphosphate glasses was studied by optical absorption and electron paramagnetic resonance spectroscopy. For this task, several model glasses were prepared. These were simple metaphosphates of alkaline earths, aluminum and zinc. The synthesized glass samples were irradiated with X-rays and with UV light from an Xe/Hg lamp. The cation-dependent differences in the structure of the phosphate glasses were found to have a great influence on the concentration of some radiation-induced defects and thus on the optical absorption. The influence of the different cations became especially distinct under UV light Irradiation due to the selective interaction of the UV light with the glass samples. Some additional phenomena were observed for the irradiated zinc and magnesium metaphosphate glasses which were not found by the previously undertaken study of complex phosphate glasses.