Scientific publications

2009
TiO2-CeO2 nanometric powders prepared by sol-gel method

Zaharescu, Maria | Wittmar, Alexandra | Teodorescu, Valentin | Andronescu, Cristian | Wittmar, Matthias | Veith, Michael

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Nanometric powders in the TiO2-CeO2 system were synthesized using sol-gel methods aiming at corrosion inhibitor preparation. The precursors employed were Ti(OiPr)4 as TiO2 source and Ce(NO3)3·6H2O or Ce(CH3CO2)3·xH2O as CeO2 source. Several parameters were varied, like the cerium precursor (cerium nitrate or cerium acetate) and the TiO2:CeO2 molar ratios. For both cerium sources binary powders with TiO2:CeO2 = 4:1 or 1:1 molar ratios were prepared. The obtained materials were dried 12 h in an oven at 100 °C and then thermally treated for 1 h at 400 °C with a heating rate of 1 °C·min-1 in order to eliminate the water and organic residues. In all cases, nanometric – predominantly amorphous – powders have been obtained which crystallized after the 1 h thermal treatment at 400 °C. The only exception was recorded for the TiO2:CeO2 = 4:1 composition prepared from the Ce(NO3)3·6H2O precursor which remained amorphous after the thermal treatment. Even though the primary particle sizes were ~ 4-5 nm, the material is constituted from aggregates larger than 50 nm. The desired presence of cerium in two valence states, necessary in active corrosion protection, was achieved and it was put into evidence by XPS and DTA/TGA for the TiO2:CeO2 = 4:1 binary compositions. Future studies have to be performed in order to reduce the agglomeration of the material.

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Zeitschrift Für Anorganische Und Allgemeine Chemie,
2009, 635, 1915-1924.

2008
Alterations in event related potentials (ERP) associated with tinnitus distress and attention

Delb, Wolfgang | Strauss, Daniel J. | Low, Yin Fen | Seidler, Harald | Rheinschmitt, A. | Wobrock, Thomas | D’Amelio, Roberto

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Tinnitus related distress corresponds to different degrees of attention paid to the tinnitus. Shifting attention to a signal other than the tinnitus is therefore particularly difficult for patients with high tinnitus related distress. As attention effects on Event Related Potentials (ERP) have been shown this should be reflected in ERP measurements (N100, phase locking). In order to prove this hypothesis single sweep ERP recordings were obtained in 41 tinnitus patients as well as 10 control subjects during a period of time when attention was shifted to a tone (attended) and during a second phase (unattended) when they did not focus attention to the tone. Whereas tinnitus patients with low distress showed a significant reduction in both N100 amplitude and phase locking when comparing the attended and unattended measurement condition a group of patients with high tinnitus related distress did not show such ERP alterations. Using single sweep ERP measurements the results of our study show, that attention in high tinnitus related distress patients is captured by their tinnitus significantly more than in low distress patients. Furthermore our results provide the basis for future neurofeedback based tinnitus therapies aiming at maximizing the ability to shift attention away from the tinnitus.

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Applied Psychophysiology and Biofeedback,
2008, 33 (4), 211-221.

Unraveling the nature of room temperature grain growth in nanocrystalline materials

Ames, Markus | Markmann, Jürgen | Karos, Rudolf | Michels, Andreas | Tschöpe, Andreas | Birringer, Rainer

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We report on the observation of real-time-resolved room temperature grain growth in nanocrystalline metals. We find that neither the time evolution of size can be modeled by standard growth theories nor are there any other systems aware to us that manifest a similar growth behaviour. We detect a transition from an initially self-similar slow growth to abnormal grain growth. Its onset seems to be associated with the simultaneous decrease of microstrain with increasing grain size. Abnormal grain growth is considered as a generic feature of nanocrystallinity but is a transient state since we observed in the late stage of coarsening, using orientational imaging microscopy, a monomodal grain size distribution. We empirically find a nonlinear-response-type of growth law which is in agreement with the observed coarsening kinetics. © 2008 Acta Materialia Inc.

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Acta Materialia,
2008, 56 (16), 4255-4266.

Enhancement of capillary forces by multiple liquid bridges

De Souza, Emerson J. | Brinkmann, M. | Mohrdieck, Camilla | Arzt, Eduard

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Capillary forces can significantly contribute to the adhesion of biological and artificial micro- and nanoscale objects. In this paper, we study numerically the effect of meniscus size on the force between two homogeneous flat plates for different contact angles. The force distance curves show excellent quantitative agreement with previous investigations. The results for n menisci of equal total liquid volume reveal interesting scaling properties and an unexpected maximum force for moderately hydrophilic surfaces (i.e., contact angles around 70°). Further, we calculate the Minimum solid-liquid area for multiple bridges, the cohesive stress (i.e., force per area) between the plates, and the work required to separate them. The results are presented in two-dimensional maps, which may be useful in the understanding of biological attachment structures and in the design of artificial contact systems.

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Langmuir,
2008, 24 (16), 8813-8820.

Capillary forces between chemically different substrates

De Souza, Emerson J. | Brinkmann, M. | Mohrdieck, Camilla | Crosby, Alfred J. | Arzt, Eduard

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Motivated by experimental results, we present numerical and analytical calculations of the capillary force exerted by a capillary bridge spanning the gap between two parallel flat plates of asymmetric wettabiltiy. Depending on whether the sum of the two contact angles is smaller or larger than 180°, the capillary force is either attractive or repulsive at small separations D between the plates. In either cases the magnitude of the force diverges as D approaches zero. The leading order of this divergence is captured by an analytical expression deduced from the geometry of the meniscus of a flat capillary bridge. The results for substrates with different wettability reveal an interesting behavior: with the sum of the contact angles fixed, the magnitude of the capillary force and the rupture separation decreases as the asymmetry in contact angles is increased. In addition, we present the rupture separation, i.e., the maximal extension of a capillary bridge, as a function of the contact angles. Our results provide an extensive picture of surface wettability effects on capillary adhesion.

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Langmuir,
2008, 24 (18), 10161-10168.

Effect of contact angle hysteresis on the measurement of capillary forces

De Souza, Emerson J. | Gao, L. | McCarthy, T. J. | Arzt, Eduard | Crosby, Alfred J.

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We conduct experimental investigations of macroscopic capillary forces between two flat rigid substrates characterized by their advancing and receding contact angles with water. Our results exhibit excellent agreement with theoretical predictions obtained by the numerical solution of the capillary equation. On the basis of this comparison, we use the measurements of the capillary force to investigate the phenomenon of contact angle hysteresis. We present examples of force measurements for surfaces that display low, moderate, and high contact angle hysteresis and compare results for a larger variety of substrates. Finally, we show that for the case of water, the role of viscosity is insignificant within the range of force and velocity measured in the present work.

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Langmuir,
2008, 24 (4), 1391-1396.

Fabrication approaches for generating complex micro- and nanopatterns on polymeric surfaces

del Campo, Aranzazu | Arzt, Eduard

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Chemical Reviews,
2008, 108 (3), 911-945.

In situ indentation testing of elastomers

Deuschle, Julia K. | Buerki, Gerhard | Deuschle, H. Matthias | Enders, Susan | Michler, Johann | Arzt, Eduard

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The development of the contact is crucial in indentation testing, yet only limited knowledge exists on the true contact size for compliant materials. In this investigation the contact evolution and the deformation behavior of polydimethylsiloxane was studied during indentation in situ inside a scanning electron microscope and by observation in a light microscope. Since detailed information on the true contact area and the amount of sink-in can be acquired from finite element analysis, simulations on the indentation process have been performed in order to complement the in situ testing. Comparison of results revealed that the contact areas calculated according to the standard Oliver-Pharr procedure deviated from the real contact size by approximately 10% for the elastomeric PDMS material. © 2008 Acta Materialia Inc.

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Acta Materialia,
2008, 56 (16), 4390-4401.

Size effect on strength and strain hardening of [111] nickel sub-micron compression pillars

Frick, Carl P. | Clark, Blythe G. | Orso, Steffen | Schneider, Andreas S. | Arzt, Eduard

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This study investigates uniaxial compression behavior of focused ion beam (FIB) manufactured [1 1 1] nickel (Ni) small-scale pillars, ranging in diameter from approximately 25 µm to below 200 nm, in order to examine the effect of crystallographic orientation on the mechanical properties. This study is unique from other micro-pillar studies in that the [1 1 1] orientation has a considerably lower Schmid factor, and has multiple slip systems available. The [1 1 1] Ni pillars show a strong increase in yield stress and work hardening with decreasing diameter. The relationship between yield stress and diameter (σy ∝d−0.69) matches well with previous small-scale pillar studies. Strain hardening, which has been inconsistently observed in other micro-pillar studies, is found to be a function of both diameter and orientation. Although the precise mechanism for hardening is unknown, transmission electron microscopy reveals dislocations throughout the pillar and into the base material suggesting that dislocation interactions and deformation below the pillar play a role in the observed strain hardening. Furthermore, a slight crystallographic rotation of the pillar is observed likely contributing to the observed mechanical properties. By exploring the role of crystallography on the plastic deformation behavior, this study provides additional insight into the nature of the size effect.

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Materials Science and Engineering A-Structural Materials Properties Microstructure and Processing,
2008, 489, 319-329.

Orientation-independent pseudoelasticity in small-scale NiTi compression pillars

Frick, Carl P. | Clark, Blythe G. | Orso, Steffen | Sonnweber-Ribic, Petra | Arzt, Eduard

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This study investigates the small-scale deformation behavior of [111], [2 10] and [00 1] NiTi shape memory alloys. In stark contrast to bulk deformation behavior, the pseudoelastic behavior of sub-micron diameter compression pillars is highly dependent on diameter and relatively independent of orientation. Transmission electron microscopy is used to investigate pillars post-compression, giving insight into the deformation mechanisms involved.

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Scripta Materialia,
2008, 59 (1), 7-10.