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Paper des Monats
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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.
Gradient Composite Replicas from Protein Crystal Layer Templates produced by Pulsed Laser Deposition
(2000)
Ti/TiN multilayer coatings with multilayer periods in the range 550 nm and a final thickness of 2 µm were deposited on steel substrates by cyclic modulation of nitrogen gas flow into the chamber of a PVD sputtering device. Coating characterization was performed by cross-sectional transmission electron microscopy, glancing-angle X-ray diffraction and instrumental indentation testing. Individual a-titanium and titanium nitride layers were always observed, although for the finer microstructures, the TiN layers were thicker than the Ti layers by a factor three. The plastic hardness of the films increased steadily with decreasing layer spacing, following a HallPetch relationship. Finally, a hardness value of 42 GPa was reached, which is similar to that of a thick TiN monolayer, prepared under the same coating conditions.
The new promoted ignition combustion test apparatus at BAM matches the requirements of ASTM test method G 124 [ASTM G 124, Standard Test Method for Determining the Combustion Behavior of Metallic Materials in Oxygen-Enriched Atmospheres, 2003] and of EIGA publication, IGC Doc 13/02/E [EIGA Gas Association Document IGC Doc 13/02/E, Oxygen Pipeline Systems, 2003]. The test apparatus is most likely the only one in Europe. The test chamber allows investigations with pure oxygen or oxygen mixtures at pressures up to 500 bar and at temperatures up to 400°C at static or flowing gas conditions. The ignition device consists of an electrical ignition wire and a promoter. IR-sensors, distributed over the whole length of the rod, measure and record the burning temperature and allow measurement of the burn rate. A video system records the experiment for visual characterization of the burning behavior. BAM test results are compared with published data. Results on investigations with coated rods are presented. Ceramic coatings seem to be a solution for the use of certain less compatible metallic materials at higher oxygen pressures.
Two different test apparatuses are used at BAM to evaluate the safety of oxygen components: First, the promoted ignition combustion test according to ASTM G 124 [1] and to EIGA IGC Doc 13/02/E [2], and second, the new metallic disk ignition test that has not been standardized yet. The standard test method ASTM G 124 allows a ranking of metallic materials for use at high pressure oxygen. However, the transfer of those test results to valves and fittings in real-life situations is rather complex. The metallic disk ignition test, developed at BAM, is more practice oriented and uses metallic disks of different thicknesses of the investigated material. A commonly used nonmetallic sealing ring is placed in front of this disk and serves as an igniter. This test array is then exposed to high pressure gaseous oxygen impacts in a standardized pneumatic impact tester according to DIN EN 1797 [3].
The wettability of the surfaces inside the microchannels of a microfluidic device is an important property considering a liquid flows through them. Contact angle measurements usually applied to test the wettability of surfaces cannot be used for an analysis of microchannel walls within microfluidic devices. A workaround is the use of surface analytical methods, which are able to reach points of interest in microchannels and may provide information on the surface chemistry established there. In calibrating these methods by using flat polymer wafers, where the contact angle can be measured as usual, data measured in real microchannels can be evaluated in terms of wetting properties. Reference wafers of bisphenol-A polycarbonate, a polymeric material that is often used in fluidic microdevice fabrication, were treated under different oxygen plasma conditions. The modified surfaces were characterized by using XPS, time of flight (ToF)-SIMS and atomic force microscope (AFM). Surface chemistry and surface topography have been correlated with contact angle measurements. In addition, effects of ageing or rinsing after plasma treatment have also been investigated.