TY - CONF A1 - Vila-Comamala, J. A1 - Diaz, A. A1 - Guizar-Sicairos, M. A1 - Gorelick, S. A1 - Guzenko, V.A. A1 - Karvinen, P. A1 - Kewish, C.M. A1 - Färm, E. A1 - Ritala, M. A1 - Mantion, Alexandre A1 - Bunk, O. A1 - Menzel, A. A1 - David, C. ED - Morawe, C. ED - Khounsary, A.M. ED - Goto, S. T1 - Characterization of a 20-nm hard X-ray focus by ptychographic coherent diffractive imaging N2 - Recent advances in the fabrication of diffractive X-ray optics have boosted hard X-ray microscopy into spatial resolutions of 30 nm and below. Here, we demonstrate the fabrication of zone-doubled Fresnel zone plates for multi-keV photon energies (4-12 keV) with outermost zone widths down to 20 nm. However, the characterization of such elements is not straightforward using conventional methods such as knife edge scans on well-characterized test objects. To overcome this limitation, we have used ptychographic coherent diffractive imaging to characterize a 20 nm-wide X-ray focus produced by a zone-doubled Fresnel zone plate at a photon energy of 6.2 keV. An ordinary scanning transmission X-ray microscope was modified to acquire the ptychographic data from a strongly scattering test object. The ptychographic algorithms allowed for the reconstruction of the image of the test object as well as for the reconstruction of the focused hard X-ray beam waist, with high spatial resolution and dynamic range. This method yields a full description of the focusing performance of the Fresnel zone plate and we demonstrate the usefulness ptychographic coherent diffractive imaging for metrology and alignment of nanofocusing diffractive X-ray lenses. T2 - SPIE Optics and photonics CY - San Diego, USA DA - 20.08.2011 KW - X-ray imaging KW - Diffractive X-ray optics KW - Electron beam lithography KW - Ptychographic coherent diffractive imaging PY - 2011 DO - https://doi.org/10.1117/12.893235 SN - 0277-786X N1 - Serientitel: Proceedings of SPIE – Series title: Proceedings of SPIE VL - 8139 SP - 81390E-1 EP - 81390E-7 AN - OPUS4-24613 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - RPRT A1 - Raupach, M. A1 - Mietz, Jürgen A1 - Nürnberger, U. A1 - Wolff, L. A1 - Bruns, M. A1 - Burkert, Andreas A1 - Eich, Gerd A1 - Menzel, K. T1 - Entwicklung eines kombinierten Schutzsystems für chloridbelastete Betonflächen aus Spritzverzinkung mit abdichtender Beschichtung (Abschlussbericht, AiF 12 818 N/2) N2 - Die Zielsetzung dieses Projektes war es, ein kombiniertes Schutzsystem aus Spritzverzinkung und abdichtendem Oberflächenschutzsystem für die Instandsetzung chloridbelasteter und korrosionsgeschädigter Stahlbetonbauteile zu entwickeln. Dabei soll die Spritzverzinkung der Betonoberfläche in den ersten Jahren nach der Instandsetzung einen kathodischen Korrosionsschutz der Bewehrung bewirken, bis der Beton infolge des Oberflächenschutzsystems soweit ausgetrocknet ist, dass auch ohne kathodischen Schutz praktisch keine Korrosion der Bewehrung mehr stattfinden kann. Anhand von Untersuchungen zur Haftung zwischen Beton, Zinkschicht und verschiedenen Oberflächenschutzsystemen wurde der Aufbau des kombinierten Schutzsystems entwickelt. Es wurden verschiedene OS-11a-Systeme ein OS-13-System sowie zwei Systeme nach ZTV-ING, Teil 7 vor und nach künstlicher Bewitterung untersucht. Anhand der Ergebnisse wurde für das kombinierte System ein OS-11a-System ausgewählt und im weiteren hinsichtlich der Wirksamkeit des kathodischen Schutzes sowie hinsichtlich der Austrocknung des Betons untersucht. Es zeigte sich sowohl an ausgelagerten Prüfköpfen sowie auf einer angelegten Versuchsfläche auf Freideck eines Parkhauses, dass ein wirksamer galvanischer kathodischer Korrosionsschutz der Bewehrung nur bei sehr hohen Chloridgehalten (4 M.-% bezogen auf den Zementgehalt) erreicht werden kann. Bei geringeren untersuchten Chloridgehalten kam es vermutlich infolge der Austrocknung der Zink/Beton-Kontaktzone nach relativ kurzer Zeit zu einer Inaktivierung des Zinks. Bei Chloridgehalten von 4 M.-% bildeten sich zwischen der Zinkschicht und dem ausgewählten OS-System gasgefüllte Blasen. Diese Problematik, sowie die Tatsache dass die Wirksamkeit des Prinzips W (Austrocknung des Betons) bei derart hohen Chloridgehalten bezweifelt werden muss, grenzt die Anwendbarkeit des Kombinationssystems mit der Zinkschicht als Opferanode deutlich ein. An neun Jahre alten, ausgelagerten Prüfköpfen durchgeführte Untersuchungen zeigten jedoch, dass mittels Fremdstrombeaufschlagung zwischen Zinkschicht und Bewehrung ein wirksamer kathodischer Schutz auch bei geringeren Chloridgehalten erreicht werden kann. Der Einsatz des entwickelten Kombinationssystems mit Fremdstrombeaufschlagung erscheint somit durchaus durchführbar. Dabei sollte der Fremdstrom jedoch vorsichtig dosiert werden, um den Haftverbund zum Zink nicht zu sehr zu schwächen. Das Ziel des Vorhabens wurde somit erreicht. KW - Chlorinduzierte Korrosion KW - Kathodischer Korrosionsschutz KW - Oberflächenschutzsystem KW - Stahlbeton KW - Thermische Spritzverzinkung PY - 2004 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-355176 SP - 1 EP - 122 PB - IBAC Institut für Bauforschung CY - Aachen AN - OPUS4-35517 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Böttger, S. A1 - Rosenberg, D. A1 - Menzel, M. A1 - Jensen, W. A1 - Busker, M. A1 - Gotlib, Z. A1 - Radtke, Martin A1 - Riesemeier, Heinrich A1 - Wobrauschek, P. A1 - Streli, C. ED - de Oliveira Guilherme Buzanich, Ana T1 - A setup for synchrotron-radiation-induced total reflection X-ray fluorescence and X-ray absorption near-edge structure recently commissioned at BESSY II BAMline N2 - An automatic sample changer chamber for total reflection X-ray fluorescence (TXRF) and X-ray absorption near-edge structure (XANES) analysis in TXRF geometry was successfully set up at the BAMline at BESSY II. TXRF and TXRF-XANES are valuable tools for elemental determination and speciation, especially where sample amounts are limited (<1 mg) and concentrations are low (ng ml⁻¹ to μg ml⁻¹). TXRF requires a well defined geometry regarding the reflecting surface of a sample carrier and the synchrotron beam. The newly installed chamber allows for reliable sample positioning, remote sample changing and evacuation of the fluorescence beam path. The chamber was successfully used showing accurate determination of elemental amounts in the certified reference material NISTwater 1640. Low limits of detection of less than 100 fg absolute (10 pg ml⁻¹) for Ni were found. TXRF-XANES on different Re species was applied. An unknown species of Re was found to be Re in the +7 oxidation state. KW - TXRF KW - TXRF-XANES KW - Sample changer KW - BAMline KW - Re-XANES PY - 2016 DO - https://doi.org/10.1107/S1600577516001995 SN - 1600-5775 VL - 23 IS - 3 SP - 820 EP - 824 PB - International Union of Crystallography AN - OPUS4-38656 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Vila-Comamala, J. A1 - Diaz, A. A1 - Guizar-Sicairos, M. A1 - Mantion, Alexandre A1 - Kewish, C.M. A1 - Menzel, A. A1 - Bunk, O. A1 - David, C. T1 - Characterization of high-resolution diffractive X-ray optics by ptychographic coherent diffractive imaging N2 - We have employed ptychographic coherent diffractive imaging to completely characterize the focal spot wavefield and wavefront aberrations of a high-resolution diffractive X-ray lens. The ptychographic data from a strongly scattering object was acquired using the radiation cone emanating from a coherently illuminated Fresnel zone plate at a photon energy of 6.2 keV. Reconstructed images of the object were retrieved with a spatial resolution of 8 nm by combining the difference-map phase retrieval algorithm with a non-linear optimization refinement. By numerically propagating the reconstructed illumination function, we have obtained the X-ray wavefield profile of the 23 nm round focus of the Fresnel zone plate (outermost zone width, Δr = 20 nm) as well as the X-ray wavefront at the exit pupil of the lens. The measurements of the wavefront aberrations were repeatable to within a root mean square error of 0.006 waves, and we demonstrate that they can be related to manufacturing aspects of the diffractive optical element and to errors on the incident X-ray wavefront introduced by the upstream beamline optics. KW - Fourier zone plate KW - Coherent diffraction imaging KW - Ptychography PY - 2011 DO - https://doi.org/10.1364/OE.19.021333 SN - 1094-4087 VL - 19 IS - 22 SP - 21333 EP - 21344 PB - Optical Society of America CY - Washington, DC AN - OPUS4-24615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Niehoff, A. A1 - Mantion, Alexandre A1 - McAloney, R. A1 - Huber, Alexandra A1 - Falkenhagen, Jana A1 - Goh, C.M. A1 - Thünemann, Andreas A1 - Winnik, M. A. A1 - Menzel, H. T1 - Elucidation of the structure of poly(gamma-benzyl-L-glutamate) nanofibers and gel networks in a helicogenic solvent N2 - The synthesis, characterization, self-assembly, and gel formation of poly(γ-benzyl-L-glutamate) (PBLG) in a molecular weight range from ca. 7,000–100,000 g/mol and with narrow molecular weight distribution are described. The PBLG is synthesized by the nickel-mediated ring-opening polymerization and is characterized by size-exclusion chromatography coupled with multiple-angle laser light scattering, NMR, and Fourier transform infrared spectroscopy. The self-assembly and thermoreversible gel formation in the helicogenic solvent toluene is investigated by transmission electron microscopy, atomic force microscopy, small-angle X-ray scattering, and synchrotron powder X-ray diffraction. At concentrations significantly below the minimum gelation concentration, spherical aggregates are observed. At higher concentrations, gels are formed, which show a 3D network structure composed of nanofibers. The proposed self-assembly mechanism is based on a distorted hexagonal packing of PBLG helices parallel to the axis of the nanofiber. The gel network forms due to branching and rejoining of bundles of PBLG nanofibers. The network exhibits uniform domains with a length of 200±42 nm composed of densely packed PBLG helices. KW - Poly(gamma-benzyl-L-glutamate) (PBLG) KW - Nickel-mediated NCA polymerization KW - Thermoreversible gel formation KW - Physical/supramolecular organogel KW - Nanofiber KW - Self-assembly KW - Alpha-helix KW - Nanotechnology KW - Small-angle X-ray scatering KW - SAXS PY - 2013 DO - https://doi.org/10.1007/s00396-012-2866-9 SN - 0303-402X SN - 1435-1536 VL - 291 IS - 6 SP - 1353 EP - 1363 PB - Springer CY - Berlin AN - OPUS4-28615 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fittschen, U.E.A. A1 - Menzel, M. A1 - Scharf, O. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Buzanich, Günter A1 - Lopez, V.M. A1 - McIntosh, K. A1 - Streli, C. A1 - Havrilla, G.J. T1 - Observation of X-ray shadings in synchrotron radiation-total reflection X-ray fluorescence using a color X-ray camera N2 - Absorption effects and the impact of specimen shape on TXRF analysis has been discussed intensively. Model calculations indicated that ring shaped specimens should give better results in terms of higher counts per mass signals than filled rectangle or circle shaped specimens. One major reason for the difference in signal is shading effects. Full field micro-XRF with a color X-ray camera (CXC) was used to investigate shading, which occurs when working with small angles of excitation as in TXRF. The device allows monitoring the illuminated parts of the sample and the shaded parts at the same time. It is expected that sample material hit first by the primary beam shade material behind it. Using the CXC shading could be directly visualized for the high concentration specimens. In order to compare the experimental results with calculation of the shading effect the generation of controlled specimens is crucial. This was achieved by 'drop on demand' technology. It allows generating uniform, microscopic deposits of elements. The experimentally measured shadings match well with those expected from calculation. KW - TXRF KW - Full field micro-XRF KW - Color X-ray camera PY - 2014 DO - https://doi.org/10.1016/j.sab.2014.06.025 SN - 0584-8547 SN - 0038-6987 VL - 99 SP - 179 EP - 184 PB - Elsevier CY - Amsterdam AN - OPUS4-31180 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Reuther, H. A1 - Menzel, Michael A1 - Vinnichenko, M. A1 - Kolitsch, A. ED - Garcia, M. T1 - Investigation of the Sn4+ Charge Density Variation in In2O3 using Mössbauer Spectroscopy T2 - International Symposium on the Industrial Application of the Mössbauer Effect CY - Madrid, Spain DA - 2004-10-04 PY - 2005 SN - 0-7354-0250-7 SN - 0094-243X N1 - Serientitel: AIP conference proceedings – Series title: AIP conference proceedings IS - 765 SP - 132 EP - 136 PB - American Inst. of Physics CY - Melville AN - OPUS4-12150 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stößer, R. A1 - Feist, M. A1 - Willgeroth, Carola A1 - Emmerling, Franziska A1 - Menzel, Michael A1 - Reuther, H. T1 - The 'quiet Goldschmidt' - a mechanochemical, thermoanalytical, and spectroscopic study of selected steps of the aluminothermic reaction N2 - The Goldschmidt reaction (2Al+α-Fe2O3) was investigated both under mechanical and thermal activation by employing a combination of analytical methods such as ESR and Mössbauer spectroscopy, magnetic susceptibility, X-ray powder diffraction, and thermal analysis (TA). Both the mechanical treatment and the TA runs under air caused the reaction conditions of 'quiet redox reactions' due to a retarding effect and enabled a reaction study in a 'slow motion mode'. This allowed to establish distinct partial steps of the integral reaction process depending on the intensity of the mechanical impact, the educt composition, the gas phase composition, and, finally, the thermal excitation in the TA runs. Particular attention was payed to the role of the gas phase and to the reaction of aluminum with differently activated oxygen species. The phlegmatizing effect was traced back to the formation of Al2O3 coverages of the Al particles. KW - Thermite reaction KW - Iron ESR and Mössbauer spectroscopy KW - Mechanochemical activation KW - Magnetic moments KW - DTA-TG KW - XRD PY - 2013 DO - https://doi.org/10.1016/j.jssc.2013.02.032 SN - 0022-4596 SN - 1095-726X VL - 202 SP - 173 EP - 190 PB - Elsevier CY - San Diego, Calif. AN - OPUS4-29528 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Renz, F. A1 - Zaba, C. A1 - Roßberg, L. A1 - Jung, S. A1 - Klein, M. A1 - Klingelhöfer, G. A1 - Wünsche, A. A1 - Reinhardt, S. A1 - Menzel, Michael T1 - Spin transition in heptanuclear star-shaped iron(III)-antimony(V) NCS- and CN-bridged compounds N2 - The precursor [FeIII(L)Cl] (LH2 = N,N'-bis(2'-hydroxy-benzyliden)-1,6-diamino-3-azahexane) has been prepared and Mössbauer spectroscopy assigned a high-spin (S = 5/2) state at room temperature. The precursor is combined with the bridging units [SbV(X)6]- (X = CN-, NCS-) to yield star-shaped heptanuclear clusters [(LFeIII-X)6SbV]Cl5. The star-shaped compounds are in general high-spin systems at room temperature. On cooling to 20 K some of the iron(III) centers switch to the low-spin state as indicated by Mössbauer spectroscopy, i.e. multiple electronic transitions. While the cyano-bridged complex performs a multiple spin transition the thiocyanate-compound shows no significant population at both temperatures. KW - Heptanuclear KW - High-spin molecule KW - SbV KW - Multistability KW - Multiple spin transition PY - 2009 DO - https://doi.org/10.1016/j.poly.2008.12.027 SN - 0277-5387 VL - 28 IS - 9-10 SP - 2036 EP - 2038 PB - Elsevier CY - Amsterdam [u.a.] ; Jena AN - OPUS4-19659 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stößer, R. A1 - Feist, M. A1 - Menzel, Michael A1 - Nofz, Marianne T1 - Fe3+ ions acting as probes and agents in aggregation processes and solid-state reactions in AlO(OH)/Al2O3 matrices N2 - The fate of doped iron species during various mechanically and thermally initiated redox reactions and aggregation processes in crystalline and amorphous AlO(OH) or Al2O3 matrices was investigated. The amorphization of the matrix was performed by chemical (i.e., via sol-gel processes) or mechanochemical treatment (high-energy ball milling). Thermal analysis, coupled with mass spectrometry (TA-MS), Mössbauer spectroscopy, and electron spin resonance (ESR), was used. The TA under various gas atmospheres allowed preparing samples under a controlled temperature regime, together with a controlled gas influence. Both the effect of mechanical activation and the influence of the iron doping could be followed macroscopically via the down-shift of the peak temperature of the corundum formation. The ESR data characterize the Fe3+ ions and their interaction with the magnetic surrounding based on the fine structure parameters. The Mössbauer data allowed the characterization of the Fe(0), Fe2+, and Fe3+ species, together with providing information about their coordinative surrounding. Both methods provided general complementary spectroscopical information. Unexpectedly, (FeOx)n and (FexAl1-x)2O3 aggregates could also be detected in the range of low Fe concentrations. It was demonstrated that even in the low-level doped systems [(FexAl1-x)2O3 with x ≥ 0.01], all the essential spectroscopic phenomena occur. At higher Fe concentrations, they were discovered to be caused by magnetic and spin exchange interactions as well as by solid-state reactions during and after the mechanical activation. PY - 2010 DO - https://doi.org/10.1111/j.1551-2916.2009.03596.x SN - 0002-7820 SN - 1551-2916 VL - 93 IS - 5 SP - 1447 EP - 1456 PB - Blackwell Publishing CY - Malden AN - OPUS4-21235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jung, S. A1 - Renz, F. A1 - Klein, M. A1 - Menzel, Michael A1 - Boca, R. A1 - Stößer, R. T1 - Molecular switching in iron complexes bridged via tincyanides observed by Mössbauer and ESR spectroscopy N2 - The precursor [FeIII(L)Cl] (LH2 = N,N'-bis(2'-hydroxy-3'-X-benzyliden)-1,6-diamino-3-N-hexane) is a high-spin (S = 5/2) complex (with X = -CH3, -O-CH3). This precursor is combined with the bridging unit [SnIV(CN)4] to yield star-shaped pentanuclear clusters, [(L-X-FeIII)4Sn(CN)4]Cl4 57Fe-Mössbauer, 119mSn-Mössbauer, and ESR spectroscopy are used to study our samples. For X = -CH3 the 57Fe-Mössbauer data show a multiple spin transition between iron(III) in the high-spin and low-spin state. Changing the functional group from X = -CH3 to X = -O-CH3 turns the switchability off. KW - Switching iron complexes KW - Spin-transition KW - Mössbauer spectroscopy KW - ESR-spectroscopy PY - 2010 DO - https://doi.org/10.1088/1742-6596/217/1/012027 SN - 1742-6588 SN - 1742-6596 VL - 217 IS - 1 / 012027 SP - 1 EP - 6 PB - IOP Publ. CY - Bristol, UK AN - OPUS4-22561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nariaki, D. A1 - Lekovic, F. A1 - Homenya, P. A1 - Costa, B. F. O. A1 - Menzel, Michael A1 - Boca, R. A1 - Blumers, M. A1 - Klingelhöfer, G. A1 - Renz, F. T1 - Iron(III) complexes on a dendrimeric basis and various amine core investigated by Mössbauer spectroscopy N2 - Dendrimers of various generations were synthesized by the divergent method. Starting from various amine cores (G0a, G0b, G0c) the generations were built by reaction of the amine with acrylnitrile followed by hydrogenation with DIBAL-H. Treatment with salicylaldehyde creates a fivefold coordination sphere for iron in the molecular periphery. The resulting multinuclear coordination compounds are investigated by Mossbauer spectroscopy. T2 - ICRTP 2014 - International conference on recent trends in physics CY - Indore, India DA - 22.02.2014 PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-316331 DO - https://doi.org/10.1088/1742-6596/534/1/012003 SN - 1742-6588 SN - 1742-6596 VL - 534 IS - 1 SP - 012003-1 EP - 012003-8 PB - IOP Publ. CY - Bristol, UK AN - OPUS4-31633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Balle, P. A1 - Geiger, B. A1 - Klukowski, D. A1 - Pignatelli, M. A1 - Wohnrau, S. A1 - Menzel, Michael A1 - Zirkwa, I. A1 - Brunklaus, G. A1 - Kureti, S. T1 - Study of the selective catalytic reduction of NOx on an efficient Fe/HBEA zeolite catalyst for heavy duty diesel engines KW - SCR KW - BEA KW - Zeolite KW - Fe KW - Active sites KW - Diesel engine KW - Hydrothermal aging KW - SO2 stability PY - 2009 DO - https://doi.org/10.1016/j.apcatb.2009.06.031 SN - 0926-3373 SN - 1873-3883 VL - 91 IS - 3-4 SP - 587 EP - 595 PB - Elsevier CY - Amsterdam AN - OPUS4-19798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stößer, R. A1 - Menzel, Michael A1 - Feist, M. A1 - Nofz, Marianne A1 - Renz, F. T1 - Competing redox reactions in Fe-containing AlO(OH) and Al2O3 matrices: A combined investigation by Mössbauer, ESR spectroscopy and thermal analysis N2 - The investigation of iron-doped AlO(OH)/Al2O3 systems revealed that the combined employment of Mössbauer and ESR spectroscopies together with thermal analysis yields meaningful data with complementary information. This mutual complementarity is based on the coexistence of Fe point defects with the corresponding aggregated FeOx species which has been observed even for very low Fe concentrations. Competing redox processes between the dopant, the AlOx matrix, and the gas atmosphere during the thermal treatment enable the generation of solid phases exhibiting specific chemical properties. The entire reaction process is influenced by a specific mechanical and thermal pre-treatment that affects predominantly oxydative processes in the matrix. A protecting influence of the matrix preventing further reductive attack of the Fe3+ Fe2+ ions by hydrogen has been established. KW - Mössbauer KW - ESR spectroscopy KW - Thermal analysis KW - Al2O3 KW - Magnetite KW - Fe(0) KW - Fe(2+) KW - Fe(3+) PY - 2010 UR - http://iopscience.iop.org/1742-6596/217/1/012028/pdf/1742-6596_217_1_012028.pdf DO - https://doi.org/10.1088/1742-6596/217/1/012028 SN - 1742-6588 SN - 1742-6596 VL - 217 IS - 1 SP - 012028-1 - 012028-5 PB - IOP Publ. CY - Bristol, UK AN - OPUS4-21876 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stößer, R. A1 - Menzel, Michael A1 - Feist, M. T1 - The fate of Fe3+ ions in the system {AlO(OH)-xerogel/Fe-compounds} after mechanical activation and different thermal treatments studied by Mössbauer, ESR spectroscopy and thermal analysis KW - Mössbauer KW - ESR KW - Thermal analysis KW - High energy ball milling KW - Activation/deactivation processes KW - Local mechano-chemical reactions KW - Heterogeneous redox reactions PY - 2009 DO - https://doi.org/10.1007/s10751-009-9920-0 SN - 0304-3843 SN - 1572-9540 VL - 190 IS - 1-3 SP - 43 EP - 49 PB - Kluwer CY - Dordrecht AN - OPUS4-19478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stößer, R. A1 - Feist, M. A1 - Patzwaldt, K. A1 - Menzel, Michael A1 - Emmerling, Franziska ED - Brooks, H. T1 - Redox reactions of K3[Fe(CN)6] during mechanochemically stimulated phase transitions of AlOOH N2 - Thermally induced redox reactions of K3[Fe(CN)6] (1) were investigated for a broad temperature range by thermal methods and structure analytical methods (ESR and Mößbauer spectroscopy, X-ray Powder diffraction and XANES). Based on the influence of the mechanically activated and transforming matrices 2 and 3, redox processes can be tuned to form doped Al2O3 systems which contain either isolated Fe3+ centres or redox active phases and precursors like (Al1-xFex)2O3 (4), (Al3-xFex)O4 (5), Fe3O4, Fe2O3 and Fe0. The phase Fe3C and the chemically reactive C-species were detected during the reaction of 1. The final composition of the doped products of α-Al2O3 is mainly influenced by the chemical nature of the Fe doping component, the applied temperature and time regime, and the composition of the gas phase (N2, N2/O2 or N2/H2). From the solid state chemistry point of view it is interesting that the transforming matrix (2 and 3) possesses both oxidative and protective properties and that the incorporation of the Fe species can be performed systematically. KW - A. Inorganic compounds KW - C. Mössbauer spectroscopy KW - C. Thermogravimetric analysis KW - D. Electron paramagnetic resonance KW - ESR-Spektroskopie KW - Kaliumhexacyanoferrat(III) KW - Mechanische Aktivierung KW - Mößbauer-Spektroskopie KW - Redoxreaktionen KW - TA-MS-Messungen PY - 2011 DO - https://doi.org/10.1016/j.jpcs.2011.03.016 SN - 0022-3697 VL - 72 IS - 6 SP - 794 EP - 799 PB - Pergamon Press CY - New York, NY AN - OPUS4-23685 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nachtigall, O. A1 - Kusserow, M. A1 - Clerac, R. A1 - Wernsdorfer, W. A1 - Menzel, Michael A1 - Renz, F. A1 - Mrozinski, J. A1 - Spandl, J. T1 - [Fe19] “Super-Lindqvist” Aggregate and Large 3D Interpenetrating Coordination Polymer from Solvothermal Reactions of [Fe2(OtBu)6] with Ethanol N2 - The syntheses, crystal structures, and physical properties of [HFe19O14(OEt)30] and {Fe11(OEt)24}1 are reported. [HFe19O14(OEt)30] has an octahedral shape. Its core with a central Fe metal ion surrounded by six m6-oxo ligands is arranged in the rock salt structure. {Fe11(OEt)24}1 is a mixedvalence coordination polymer in which FeIII metal ions form three 3D interpenetrating (10,3)-b nets. The arrangement of the FeIII ions can also be compared to that of Si ions in a-ThSi2. Thus, the described structures are at the interface between molecular and solid-state chemistry. KW - Solvothermal syntheses KW - Coordination polymers KW - Koordinationspolymere KW - Iron KW - Eisen KW - Polyoxometalates KW - Single-molecule magnets KW - Einzelmolekülmagnete PY - 2015 DO - https://doi.org/10.1002/anie.201503647 VL - 54 SP - 10361 EP - 10364 PB - Wiley-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-35368 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kolb, U. A1 - Büscher, K. A1 - Helm, C.A. A1 - Lindner, A. A1 - Thünemann, Andreas A1 - Menzel, Michael A1 - Higuchi, M. A1 - Kurth, D.G. T1 - The solid-state architecture of a metallosupramolecular polyelectrolyte N2 - Self-assembly of Fe(II) and the ditopic ligand 1,4-bis(2,2':6',2"-terpyridine-4'-yl)benzene results in equilibrium structures in solutions, so-called metallosupramolecular coordination polyelectrolytes (MEPEs). It is exceedingly difficult to characterize such macromolecular assemblies, because of the dynamic nature. Therefore, hardly any structural information is available for this type of material. Here, we show that from dilute solutions, where small aggregates predominate, it is possible to grow nanoscopic crystals at an interface. A near atomic resolution structure of MEPE is obtained by investigating the nanoscopic crystals with electron diffraction in combination with molecular modeling. The analysis reveals a primitive monoclinic unit cell (P21/c space group, a = 10.4 Å, b = 10.7 Å, c = 34.0 Å, α = γ = 90°, β = 95°, ρ = 1.26 g/cm³, and Z = 4). The MEPE forms linear rods, which are organized into sheets. Four sheets intersect the unit cell, while adjacent sheets are rotated by 90° with respect to each other. The pseudooctahedral coordination geometry of the Fe(II) centers is confirmed by Mössbauer spectroscopy. The combination of diffraction and molecular modeling presented here may be of general utility to address problems in structural materials science. KW - Polymer KW - Polyelectrolyte KW - Electron diffraction KW - Mössbauer spectroscopy KW - Molecular modeling KW - Supramolecular chemistry PY - 2006 SN - 0027-8424 SN - 1091-6490 VL - 103 IS - 27 SP - 10202 EP - 10206 PB - National Academy of Sciences CY - Washington, DC AN - OPUS4-12495 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Renz, F. A1 - Jung, S. A1 - Klein, M. A1 - Menzel, Michael A1 - Thünemann, Andreas T1 - Molecular switching complexes with iron and tin as central atom N2 - The precursor [FeIII(L)Cl] (LH