TY - JOUR A1 - Bennet, Francesca A1 - Opitz, R. A1 - Ghoreishi, N. A1 - Plate, K. A1 - Barnes, J.-P. A1 - Bellew, A. A1 - Bellu, A. A1 - Ceccone, G. A1 - de Vito, E. A1 - Delcorte, A. A1 - Franquet, A. A1 - Fumageli, F. A1 - Gilliland, D. A1 - Jungnickel, H. A1 - Lee, T.G. A1 - Poleunis, C. A1 - Rading, D. A1 - Shon, H.K. A1 - Spampinato, V. A1 - Son, J.G. A1 - Wang, F. A1 - Wang, Y.-C. A. A1 - Zhao, Y. A1 - Roloff, A. A1 - Tentschert, J. A1 - Radnik, Jörg T1 - VAMAS TWA2 interlaboratory comparison: Surface analysis of TiO2 nanoparticles using ToF-SIMS JF - Journal of Vacuum Science and Technology A N2 - Due to the extremely high specific surface area of nanoparticles and corresponding potential for adsorption, the results of surface analysis can be highly dependent on the history of the particles, particularly regarding sample preparation and storage. The sample preparation method has, therefore, the potential to have a significant influence on the results. This report describes an interlaboratory comparison (ILC) with the aim of assessing which sample preparation methods for ToF-SIMS analysis of nanoparticles provided the most intra- and interlaboratory consistency and the least amount of sample contamination. The BAM reference material BAM-P110 (TiO2 nanoparticles with a mean Feret diameter of 19 nm) was used as a sample representing typical nanoparticles. A total of 11 participants returned ToF-SIMS data,in positive and (optionally) negative polarity, using sample preparation methods of “stick-and-go” as well as optionally “drop-dry” and “spin-coat.” The results showed that the largest sources of variation within the entire data set were caused by adventitious hydrocarbon contamination or insufficient sample coverage, with the spin-coating protocol applied in this ILC showing a tendency toward insufficient sample coverage; the sample preparation method or the participant had a lesser influence on results. KW - Secondary Ion Mass Spectrometry KW - VMAAS KW - Titania KW - Interlaboratory comparison KW - Reproducibility PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582290 DO - https://doi.org/10.1116/6.0002814 SN - 0734-2101 VL - 41 IS - 5 SP - 053210-1 EP - 053210-13 PB - AIP (American Institute of Physics) AN - OPUS4-58229 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brzezinka, Klaus-Werner A1 - Trunschke, A. A1 - Hoang, D. L. A1 - Radnik, J. A1 - Brückner, A. A1 - Lieske, H. T1 - Transition metal oxide/carbon composite catalysts for n-alkane aromatization: Structure and catalytic properties JF - Applied catalysis / A N2 - Nanocrystalline particles of high temperature pretreated titania, zirconia or hafnium oxide, embedded in a carbon matrix, have been found to catalyze the aromatization of n-octane into ethylbenzene (EB) and o-xylene (OX) with high selectivity. The carbon matrix itself is catalytically not active, but seems to co-operate with the transition metal oxides in such a way that the various metal oxide/carbon composite materials exhibit equal selectivity patterns. In detail, the carbon component stabilizes a high dispersion of the oxides during the high temperature pretreatment procedure. This thermal treatment results in a destruction of surface acidity of the oxides, which would otherwise be responsible for undesirable consecutive and parallel reactions. Moreover, the carbon component is involved in the deep dehydrogenation of alkanes to multiple unsaturated alkenes. This is explained by the ability of surface carbon atoms to interact with hydrogen. The bulk and surface structure of the catalysts have been characterized by XRD, specific surface area measurements, XPS, UPS, Raman spectroscopy, in situ ESR and DRIFT spectroscopy. KW - Aromatization KW - Dehydrocyclization KW - n-Octane KW - Monofunctional catalysts KW - Zirconia KW - Titania KW - Oxide/carbon composites PY - 2001 DO - https://doi.org/10.1016/S0926-860X(00)00736-5 SN - 0926-860X SN - 1873-3875 VL - 208 IS - 1-2 SP - 381 EP - 392 PB - Elsevier CY - Amsterdam AN - OPUS4-1083 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grulke, E. A. A1 - Yamamoto, K. A1 - Kumagai, K. A1 - Häusler, Ines A1 - Österle, Werner A1 - Ortel, Erik A1 - Hodoroaba, Vasile-Dan A1 - Brown, S. C. A1 - Chan, C. A1 - Zheng, J. A1 - Yamamoto, K. A1 - Yashiki, K. A1 - Song, N. W. A1 - Kim, Y. H. A1 - Stefaniak, A. B. A1 - Schwegler-Berry, D. A1 - Coleman, V. A. A1 - Jämting, Å. K. A1 - Herrmann, J. A1 - Arakawa, T. A1 - Burchett, W. W. A1 - Lambert, J. W. A1 - Stromberg, A. J. T1 - Size and shape distributions of primary crystallites in titania aggregates JF - Advanced Powder Technology N2 - The primary crystallite size of titania powder relates to its properties in a number of applications. Transmission electron microscopy was used in this interlaboratory comparison (ILC) to measure primary crystallite size and shape distributions for a commercial aggregated titania powder. Data of four size descriptors and two shape descriptors were evaluated across nine laboratories. Data repeatability and reproducibility was evaluated by analysis of variance. One-third of the laboratory pairs had similar size descriptor data, but 83% of the pairs had similar aspect ratio data. Scale descriptor distributions were generally unimodal and were well-described by lognormal reference models. Shape descriptor distributions were multi-modal but data visualization plots demonstrated that the Weibull distribution was preferred to the normal distribution. For the equivalent circular diameter size descriptor, measurement uncertainties of the lognormal distribution scale and width parameters were 9.5% and 22%, respectively. For the aspect ratio shape descriptor, the measurement uncertainties of the Weibull distribution scale and width parameters were 7.0% and 26%, respectively. Both measurement uncertainty estimates and data visualizations should be used to analyze size and shape distributions of particles on the nanoscale. KW - Measurement uncertainty KW - Size distribution KW - Shape distribution KW - TEM KW - Titania PY - 2017 DO - https://doi.org/10.1016/j.apt.2017.03.027 SN - 0921-8831 VL - 28 IS - 7 SP - 1647 EP - 1659 PB - Elsevier B.V. AN - OPUS4-40478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hübert, Thomas A1 - Unger, Brita A1 - Bücker, Michael T1 - Sol-gel derived TiO2 wood composites JF - Journal of sol gel science and technology N2 - The sol–gel process was applied to enhance properties of pine sapwood. For this purpose wood prisms were soaked in nanoscaled precursor solutions prepared from titanium(IV) n-butoxide and titanium(IV) iso-propoxide, respectively, using vacuum impregnation technique. The wet composites were cured by special program with final heat treatment at 103 °C. Weight percent gains (WPG) of the wood specimen in the range of 19-25% were obtained due to these procedures. SEM investigations show that precursor solutions penetrate into the whole wood body and the titania formed after heat treatment in the composites is deposited in the pores (lumen) and partly in the cell walls of the wooden matrix. The moisture sorption was investigated in long term tests for a period of some months by storage at 20-23 °C in humid air (relative humidity of 99%) and ambient atmosphere (relative humidity 40-60%), respectively. For untreated reference samples the moisture sorption results in increasing of mass and volume according to saturation values of 24 and 13%, respectively, after about 15 days. The incorporation of titania reduces the saturation values of the moisture sorption by up to 12% in mass and by up to 5% in volume at a relative humidity of 99%. Thus, an enhancement of the dimensional stability of about 60% is obtained at best. The results demonstrate that modification of wood with sol-gel derived precursors can enhance its dimensional stability, which prevents the formation of cracks. Because of that reduced moisture sorption biological attacks should be delimited. Additionally, thermal analyses show a retarded combustion of the wood matrix due to titania infiltration. KW - Titania KW - Sol-gel KW - Nanocomposites KW - Wood protection KW - Water sorption PY - 2010 DO - https://doi.org/10.1007/s10971-009-2107-y SN - 0928-0707 SN - 1573-4846 VL - 53 IS - 2 SP - 384 EP - 389 PB - Kluwer Academic Publ. CY - Dordrecht AN - OPUS4-20892 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Woydt, Mathias T1 - Tribological characteristics of polycrystalline Magnéli-type titanium dioxides JF - Tribology letters N2 - The results presented in this paper have clarified experimentally, that titania-based Magnéli-phases (Ti4O7/Ti5O9 and Ti6O11) with (121)-shear planes exhibit more anti-wear properties than lubricious (low-frictional) properties. The results for dry sliding indicate that the coefficients of friction lie in the range of 0.1–0.6 depending on sliding speed and ambient temperature. The COF decreased with increasing temperature (T= 22–800°C) and increasing sliding speed (?= 1-6 m/s). The dry sliding wear rate was lowest for the Al2O3 at 1 m/s at 800°C with values of 1.7 × 10-8 and 6.4 × 10-8 mm3/N m, comparable to boundary/mixed lubrication, associated with a high dry frictional power loss of 30 W/mm2. The running-in wear length and, more important, the wear rate decreased under oscillating sliding tests with increasing relative humidity. The contact pressure for high-/low-wear transition increased under oscillating sliding tests with increasing relative humidity. At room temperature and a relative humidity of 100% the steady-state wear rate under dry oscillating sliding for the couple Al2O3/Ti4O7–Ti5O9 was lower than 2 × 10-7 mm3/N m and therefore inferior to the resolution of the continuous wear measurement sensor. TEM of wear tracks from oscillating sliding revealed at room temperature a work-hardening as mechanism to explain the running-in behavior and the high wear resistance. The hydroxylation of titania surfaces favours the high-/low-wear transition. KW - Magnéli-phases KW - Shear planes KW - Planar defects KW - Ceramics KW - Dry friction KW - High temperature KW - Titania KW - Wear KW - Work-hardening KW - TEM KW - Humidity PY - 2000 DO - https://doi.org/10.1023/A:1019170831371 SN - 1023-8883 SN - 1573-2711 VL - 8 SP - 117 EP - 130 PB - Springer Science Business Media B.V. CY - Dordrecht AN - OPUS4-2443 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -