TY - JOUR A1 - Handrea-Haller, Marlene A1 - Sahre, Mario A1 - Kautek, Wolfgang A1 - Neubauer, A. A1 - Sleytr, U.B. T1 - Electrochemistry of nano-scale bacterial surface protein layers on gold N2 - The mechanism of the recrystallization of nano-scale bacterial surface protein layers (S-layers) on solid substrates is of fundamental interest in the understanding and engineering of biomembranes and e.g. biosensors. In this context, the influence of the charging state of the substrate had to be clarified. Therefore, the electrochemical behaviour of the S-layers on gold electrodes has been investigated by in-situ electrochemical quartz microbalance (EQMB) measurements, scanning force microscopy (SFM) and small-spot X-ray photoelectron spectroscopy (SS-XPS) of potentiostatically emersed substrates. It was shown that the negatively charged bonding sites of the S-layer units (e.g. carboxylates) can bond with positively charged Au surface atoms in the positively charged electrochemical double layer region positive of the point of zero charge (not, vert, similar-0.8 V vs. saturated mercury-mercurous sulphate electrode). Surface conditions in other potential regions decelerated the recrystallization and fixation of S-layers. Time-resolved in-situ and ex-situ measurements demonstrated that two-dimensional S-layer crystal formation on gold electrodes can occur within few minutes in contrast to hours common in self-assembled monolayer (SAM) generation. These results proved that the recrystallization and fixation of 2D-crystalline S-layers on an electronic conductor can be influenced and controlled by direct electrochemical manipulation. KW - S-layers crystallization KW - Gold KW - Electrochemical quartz microbalance KW - Scanning force microscopy KW - XPS PY - 2003 DO - https://doi.org/10.1016/S1567-5394(03)00047-1 SN - 0302-4598 SN - 1567-5394 VL - 61 SP - 1 EP - 8 PB - Elsevier Science CY - Oxford AN - OPUS4-2844 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoang, D. L. A1 - Dittmar, A. A1 - Schneider, M. A1 - Trunschke, A. A1 - Lieske, H. A1 - Brzezinka, Klaus-Werner A1 - Witke, Klaus T1 - Evidence of lanthanum-chromium mixed oxides formed in CrOx/La2O3 model catalysts N2 - CrOx/La2O3 mixed oxides, prepared by impregnating La2O3 with appropriate aqueous solutions of (NH4)2CrO4 and calcining at 600 °C for 4 h, have been investigated by means of XRD, TPR, XPS, DRIFTS, and Raman spectroscopy (RS). The formation of the compounds La2CrO6, La(OH)CrO4 and LaCrO4 under these conditions was evidenced. Strong peaks at 864, 884, 913, and 921 cm-1, as well as weak peaks at 136, 180, 354, 370, and 388 cm-1 in the RS spectrum of CrOx/La2O3 have been assigned to La2CrO6. KW - Lanthanum-chromium mixed oxides KW - La2CrO6 KW - LaCrO4 KW - TPR KW - XPS KW - XRD KW - DRIFTS KW - Raman spectroscopy PY - 2003 DO - https://doi.org/10.1016/S0040-6031(02)00491-4 SN - 0040-6031 SN - 1872-762X VL - 400 SP - 153 EP - 163 PB - Elsevier CY - Amsterdam AN - OPUS4-2397 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Österle, Werner A1 - Dörfel, Ilona A1 - Urban, Ingrid A1 - Reier, T. A1 - Schultze, J. T1 - XPS and XTEM study of AlN formation by N+2 implantation of aluminium N2 - X-ray photoelectron spectroscopy (XPS) and cross-sectional transmission electron microscopy (XTEM) were used to study the formation of AlN films by N+2 ion implantation of aluminium at energies of 3 keV and 100 keV. In both cases, a two-stage mechanism was found, comprising first the oriented precipitation of small particles of the hexagonal AlN-phase, followed by growth and coalescence finally forming a continuous AlN-layer while increasing the implantation dose from 1×1017 cm-2 to 2×1017 cm-2. The results of both methods are in excellent agreement and furthermore provide complementary information concerning chemical composition and binding energies as well as microstructural details. KW - AIN KW - Aluminium KW - N2+ KW - Implantation KW - XPS KW - XTEM PY - 1998 DO - https://doi.org/10.1016/S0257-8972(98)00355-7 SN - 0257-8972 VL - 102 IS - 1-2 SP - 168 EP - 174 PB - Elsevier Science CY - Lausanne AN - OPUS4-2363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gross, Thomas A1 - Retzko, Iris A1 - Friedrich, Jörg Florian A1 - Unger, Wolfgang T1 - Time-of-flight-SIMS and XPS characterization of metal doped polymers N2 - Organic thin films with defined chemical structures and physical properties are required for various applications. Plasma polymerization is of technological interest, since the deposition of plasma polymers is possible on any material of any shape in the desired thickness. We report on the TOF-SIMS (TOF: time-of-flight) and XPS investigations of pulse plasma ‘poly(acetylene)’ and alkali metal doped pulse plasma ‘poly(acetylene)’ films. The combination of TOF-SIMS and XPS supplies detailed information on the surface chemistry of these films. Application of both methods provides the possibility for cross-checking certain results. Moreover the different sensitivities of the methods can be utilized. According to the TOF-SIMS and XPS data it can be concluded that the interaction of alkali metals with plasma ‘poly(acetylene)’ results in electrovalent bonds of the type Me?+–C?- between carbon and metal. Furthermore carbon–oxygen–metal interactions were observed. These interactions are of the type C=O?-cdots, three dots, centeredMe?+ and/or C–O?-–Me?+. KW - SIMS KW - TOF-SIMS KW - XPS KW - Plasma KW - Polymer KW - Poly(acetylene) PY - 2003 DO - https://doi.org/10.1016/S0169-4332(02)00769-9 SN - 0169-4332 SN - 1873-5584 VL - 203-204 SP - 575 EP - 579 PB - North-Holland CY - Amsterdam AN - OPUS4-2271 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoang, D. L. A1 - Dittmar, A. A1 - Radnik, J. A1 - Witke, Klaus A1 - Brzezinka, Klaus-Werner T1 - Redox behaviour of La-Cr compounds formed in CrOX/La2O3 mixed oxides and CrOX/La2O3/ZrO2 catalysts N2 - The redox behaviour of chromium oxide in CrOx/La2O3, CrOx/La2O3/ZrO2 and CrOx/ZrO2 mixed oxide systems has been investigated by temperature-programmed reduction (TPR), photoelectron spectroscopy (XPS) and Raman spectroscopy (RS). The formation of La-Cr compounds such as La2CrO6, LaCrO4 was shown to occur by calcination of CrOx/La2O3 and CrOx/La2O3/ZrO2 at 600 °C. With a Cr content of ca. 4 wt.%, it was revealed that, having been reduced to Cr3+-containing compounds, La2CrO6 and/or LaCrO4 in both systems may be restored by reoxidation at 600 °C. In the case of CrOx/La2O3/ZrO2 catalysts, it is suggested that these compounds were real surface species anchored as an overlayer on zirconia. Such a structure may stabilise, on the one hand, the tetragonal modification of zirconia and, on the other hand, highly dispersed state of Cr species in calcined as well as in reduced catalysts. KW - Chromia containing catalysts KW - Redox reversibility KW - La-Cr compounds KW - Temperature-programmed reduction KW - XPS KW - Raman spectroscopy PY - 2003 DO - https://doi.org/10.1016/S0926-860X(02)00375-7 SN - 0926-860X SN - 1873-3875 VL - 239 IS - 1-2 SP - 95 EP - 110 PB - Elsevier CY - Amsterdam AN - OPUS4-2260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Handrea-Haller, Marlene A1 - Sahre, Mario A1 - Neubauer, A. A1 - Sleytr, U.B. A1 - Kautek, Wolfgang T1 - Electrochemistry of Nano-Scale Bacterial Surface Protein Layers on Gold KW - S-layers crystallization KW - Gold KW - Electrochemical quartz microbalance KW - Scanning force microscopy KW - XPS PY - 2002 SN - 0013-4686 SN - 1873-3859 N1 - Geburtsname von Handrea-Haller, Marlene: Handrea, M. - Birth name of Handrea-Haller, Marlene: Handrea, M. PB - Elsevier Science CY - Kidlington AN - OPUS4-1736 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schröder, K. A1 - Meyer-Plath, Asmus A1 - Keller, D. A1 - Ohl, A. T1 - On the Applicability of Plasma Assisted Chemical Micropatterning to Different Polymeric Biomaterials N2 - A plasma process sequence has been developed to prepare chemical micropatterns on polymeric biomaterial surfaces. These patterns induce a guided localized cell layover at microscopic dimension. Two subsequent plasma steps are applied. In the first functionalization step a microwave ammonia plasma introduces amino groups to obtain areas for very good cell adhesion; the second passivation step combines pattern generation and creation of cell repelling areas. This downstream microwave hydrogen plasma process removes functional groups and changes the linkages of polymer chains at the outermost surfaces. Similar results have been obtained on different polymers including polystyrene (PS), polyhydroxyethylmethacrylate (PHEMA), polyetheretherketone (PEEK), polyethyleneterephthalate (PET) and polyethylenenaphthalate (PEN). Such a rather universal chemical structuring process could widen the availability of biomaterials with specific surface preparations. KW - Microwave plasma KW - Ammonia KW - Hydrogen KW - Polymer surface KW - Cell culture KW - XPS KW - Fluorescence PY - 2002 DO - https://doi.org/10.1023/A:1016239302194 SN - 1084-0184 SN - 1572-8978 VL - 7 IS - 2 SP - 103 EP - 125 PB - Plenum Press CY - New York, NY AN - OPUS4-1729 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gross, Thomas A1 - Unger, Wolfgang A1 - Patscheider, J. T1 - Quantitative surface chemical analysis of stainless steel 1.4301 using Surface Science Instruments XPS spectrometers: report on an interlaboratory comparison N2 - Results of an interlaboratory comparison of XPS data obtained with stainless steel are presented. Only one photoelectron spectrometer model was used. The stainless-steel sample surfaces were analysed in different states by XPS: as received, after sputtering to I(C 1s)/I(Fe 2p3/2) 0.025 and after removing a chromium-enriched oxide layer following a certain protocol. The Fe, Cr and Ni elemental concentrations were evaluated from the respective XPS data submitted by the participants of the interlaboratory test experiment. Total means, repeat standard deviations (sr) and reproducibility standard deviations (sR) are presented. The best reproducibility standard deviations were obtained for the XPS analysis after removal of a chromium-enriched oxide layer and quantification of the XPS intensities without taking the contamination elements of carbon and oxygen into account. The absolute reproducibility standard deviation of the elemental concentrations in that case is as small as 1.1-1.5 at.%. This gives 2%, 6% and 16% for the relative reproducibility standard deviation of the concentrations of iron, chromium and nickel, respectively. The total means of the iron, chromium and nickel concentrations finally obtained agree within 2sR with bulk values determined by wavelength-dispersive x-ray fluorescence spectroscopy. Comparison to an earlier interlaboratory test experiment shows that using only one model of photoelectron spectrometer reduces the reproducibility standard deviations efficiently. Copyright © 2002 John Wiley & Sons, Ltd. KW - XPS KW - ESCA KW - Quantitative surface chemical analysis KW - Stainless steel KW - Interlaboratory comparison PY - 2002 DO - https://doi.org/10.1002/sia.1229 SN - 0142-2421 SN - 1096-9918 VL - 33 IS - 5 SP - 426 EP - 432 PB - Wiley CY - Chichester AN - OPUS4-1409 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unger, Wolfgang A1 - Gross, Thomas A1 - Lippitz, Andreas A1 - Güttler, B. T1 - Uncertainty in measurement of overlayer thickness of thermally oxidized silicon using x-ray photoelectron spectroscopy N2 - Overlayers of SiO2 (nominally 4, 6 and 8 nm thick) on silicon, prepared by thermal oxidation, were investigated using x-ray photoelectron spectroscopy (XPS). The thickness of these overlayers was obtained from a measurement of the photoelectron intensities originating from the substrate and the oxide overlayer by applying an appropriate quantitative model. The uncertainty budget of that thickness measurement method is given. The relative combined standard uncertainty of the method was found to be 15%. The effective attenuation lengths or the corresponding electron inelastic mean free paths are of considerable importance for both the estimated values of overlayer thickness and combined standard uncertainties. The XPS results were compared with ellipsometry data. KW - XPS KW - ESCA KW - Uncertainty KW - Overlayer KW - SiO2 PY - 2000 DO - https://doi.org/10.1002/1096-9918(200012)29:12<891::AID-SIA943>3.0.CO;2-A SN - 0142-2421 SN - 1096-9918 IS - 29 SP - 891 EP - 894 PB - Wiley CY - Chichester AN - OPUS4-1075 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg Florian A1 - Koprinarov, Ivaylo A1 - Giebler, Rainer A1 - Lippitz, Andreas A1 - Unger, Wolfgang T1 - Reactions and Intermediates at the Metal-Polymer Interface as Observed by XPS and NEXAFS Spectroscopy KW - XPS KW - NEXAFS KW - Interfacial polymer-metal redox reactions KW - Chromium-polymer intermediates KW - Near edge X-ray absorption fine structure spectroscopy KW - Adhesion KW - Polymer-metal bonds KW - Polymer-aluminium bonds KW - Polymer-copper bonds PY - 1999 SN - 0021-8464 SN - 1545-5823 VL - 71 SP - 297 EP - 321 PB - Gordon & Breach CY - New York, NY AN - OPUS4-798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -