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P Müller-Buschbaum

Publications and source records attributed to P Müller-Buschbaum.

9 recordsLinked to original sources

Surface versus confinement induced morphology transition in triblock copolymer films: a grazing incidence small angle neutron scattering investigation.

The internal nanostructure resulting from microphase separation in triblock copolymer films of polyparamethylstyrene-block-polystyrene-block-polyparamethylstyrene, P(pMS-b-Sd8-b-pMS), has been investigated with grazing incidence small angle neutron scattering (GISANS). X-ray reflectivity, grazing incidence small-angle X-ray scattering (GISAXS), optical microscopy and atomic force microscopy (AFM) complement the investigation. The influence of two limiting interfaces present in confinement is compared to the presence of only one surface. GISANS allows for the detection of structures in the very limited sample volume of confined films as well as for a depth sensitivity to probe the near free surface part of bulk films. With respect to the surface a perpendicular oriented lamella is observed. In contrast to the shrinkage of the characteristic lamellar spacing in confinement at the free surface, a slight increase is determined.

Journal Article↗

Thin casein films as prepared by spin-coating: influence of film thickness and of pH.

Casein films were successfully prepared with the spin-coating technique of aqueous casein solutions on base-treated glass surfaces. The film structure is investigated in real space with optical microscopy and atomic force microscopy and for the first time in reciprocal space with grazing incidence small-angle X-ray scattering (GISAXS). The size of the substructures detected in the film increases with pH from 170 nm (pH 5.1) up to 490 nm (pH 9.4). Dynamic light scattering experiments reveal that the average diameters of casein micelles in solution exhibit the same quantitative increase. This result suggests that the substructures detected in the bulklike films with GISAXS reflect intact casein micelles. However, with thin homogeneous casein films, the micelle size diminishes with decreasing film thickness. This indicates that the moderate pressures introduced by spin-coating force the micelles to rearrange into a more compact structure.

Caseins↗

Self-supported particle-track-etched polycarbonate membranes as templates for cylindrical polypyrrole nanotubes and nanowires: an X-ray scattering and scanning force microscopy investigation.

Self-supported particle-track-etched polycarbonate membranes with nearly perfect cylindrical pores are used for the preparation of similarly perfect cylindrical polypyrrole nanowires and nanotubes. A complete investigation of the structural properties that result at different stages of the preparation route of polypyrrole nanowires and nanotubes is based on a combination of real and reciprocal space techniques. Nanoporous membranes with nominal pore size ranging from 5 to 150 nm and pore density up to 10(9) pores/cm(2) made from 21-microm-thick polycarbonate films are used. Polypyrrole nanotubes or nanowires are synthesized inside the pores. A real-space picture of the nanomaterial results from scanning force microscopy (SFM) on ultrathin sections made in two directions to obtain structures in the sample surface as well as perpendicular to the surface. From a model-based fit to the small-angle and ultra-small-angle X-ray scattering (SAXS/USAXS) data, the geometric pore structure is obtained and compared to values determined with scanning electron microscopy (SEM). Nanopores, nanowires, and nanotubes are described by uniform solid cylinders or hollow tubes, which are oriented highly parallel to each other and exhibit a small size distribution. Below a critical pore diameter, solid nanowires are produced whereas above this limit hollow nanotubes result.

Microscopy, Atomic Force↗

Supported particle track etched polyimide membranes: a grazing incidence small-angle X-ray scattering study.

Particle track etched polyimide membranes on silicon substrates covered with a native oxide layer are investigated. Preparation steps similar to the common classical particle track etched membrane production, giving rise to free-standing membranes, are successfully applied to the supported membranes. Polyimide films are used as a starting material for a template preparation based on high energy ion irradiation. The film/membrane structure is probed at different length scales by grazing incidence small-angle X-ray scattering at each individual preparation step. In addition, characterization with atomic force microscopy, variable-angle spectroscopic ellipsometry, Fourier transform infrared transmission, and attenuated total reflection spectroscopy is performed. An amount of 6 +/- 1 vol % pores inside the polyimide film is detected. The pores are oriented perpendicular to the substrate surface and have a conical shape, yielding a slightly reduced pore size at the substrate/film interface.

Journal Article↗

Influence of surface cleaning on dewetting of thin polystyrene films.

Thin polystyrene (PS) films on top of silicon substrates are a frequently investigated model system in the framework of unstable films. However, with respect to stability the various experiments yielded contradictory results. Focussing on the influence of preparation conditions such as the surface cleaning solves these contradictions. By applying different surface cleans the PS film can be changed from a stable homogeneous one into a completely dewetted one. In addition to the type of clean applied, the time between cleaning the surface and spin-coating the polymeric layer on top turned out to be an important experimental parameter.

Journal Article↗

Photon correlation spectroscopy with high-energy coherent x rays.

We performed x-ray photon correlation spectroscopy on a model suspension of colloidal particles using x rays of three different energies, namely, 8 keV, 13.5 keV, and 19 keV. The observed reduction in the degree of coherence with increasing x-ray energy, as measured by the contrast of the correlation functions, is consistent with theoretical estimates. We show that it is well possible and under certain circumstances even advantageous to perform experiments with coherent x rays at these higher energies. We argue that the reduced absorption may not only allow for thicker samples but also for longer acquisition times because of the reduced radiation damage, thus outweighing in many cases the effect of the reduced coherent flux. The use of higher energy x rays for photon correlation spectroscopy can therefore lead to a substantial increase in the signal-to-noise ratio and constitutes a promising option for future experiments on samples of polymeric or biological origin.

Models, Theoretical↗

Grazing incidence small-angle X-ray scattering: an advanced scattering technique for the investigation of nanostructured polymer films.

Hamburg workshop on the "application of synchrotron radiation in chemistry"With grazing incidence small-angle X-ray scattering (GISAXS) the limitations of conventional small-angle X-ray scattering with respect to extremely small sample volumes in the thin-film geometry are overcome. GISAXS turned out to be a powerful advanced scattering technique for the investigation of nanostructured polymer films. Similar to atomic force microscopy (AFM), a large interval of length between molecular and mesoscopic scales is detectable with a surface-sensitive scattering method. While with AFM only surface topographies are accessible, with GISAXS the buried structure is also probed. Because a larger surface area is probed, GISAXS also has a much larger statistical significance compared to AFM. Due to the high demand on collimation, GISAXS experiments are based on synchrotron radiation. Nanostructures parallel and perpendicular to the sample surface observable in thin poly(styrene- block-isoprene) diblock copolymer films are presented as an example of the possibilities of GISAXS.

Journal Article↗

Phase Separation and Dewetting of Weakly Incompatible Polymer Blend Films.

The phase separation and dewetting of thin films of blends of deuterated polystyrene (dPS) and poly(p-methylstyrene) (PpMS) were investigated during annealing. The surface morphology, obtained from atomic force microscopy and phase measurement interference microscopy, the density profile, determined by X-ray reflectivity in the region of total external reflection, and the surface composition obtained from static secondary ion mass spectroscopy, are reported. This system is only weakly incompatible. The interaction of the components with substrate and air during phase separation leads to a bilayer formation with a broad polymer-polymer interface. PpMS segregates to the air interface. The bilayer structure is unstable and defines the starting point for the dewetting of PpMS on top of the dPS layer. In the final dewetting state a homogeneous layer of dPS on top of the substrate is covered with an ultrathin layer of PpMS as well as with quite thick mesoscopic drops of PpMS.

Journal Article↗