Determination of micrometer length scales with an X-ray reflection ultra small-angle scattering set-up

Müller‐Buschbaum, Peter; Casagrande, M.; Gutmann, Jochen S.; Kuhlmann, T.; Stamm, Manfred; Krosigk, G. von; Lode, U.; Cunis, S.; Gehrke, Rainer

doi:10.1209/epl/i1998-00282-0

Cited by 41 publications

(46 citation statements)

References 17 publications

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“…The two-dimensional intensity distribution separated in several vertical and horizontal slices was detected at a fixed angle of incidence α i . On the one hand the vertical slices [33] correspond to detector scans, which are mainly dependent on q z and include depth sensitive information [34] On the other hand the horizontal slices corresponding to so-called out-of-plane scans include in-plane information of the most prominent lateral size from q y dependence. The horizontal slices were taken at the angle α= α i + α c , where α c is the critical angle of total reflection for the polyampholyte At this position the horizontal slices include the contribution of lateral sizes in the adsorbed polyampholyte layer.…”

Section: Scanning Force Microscopymentioning

confidence: 99%

Highly Regular Polyampholytic Structures Adsorbed Directly from Solution

Mahltig

Müller‐Buschbaum

Wolkenhauer

et al. 2001

Journal of Colloid and Interface Science

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This article concerns the adsorption of the diblock polyampholyte poly(methacrylic acid)-blockpoly((dimethylamino)ethyl methary-late) (PMAA-b-PDMAEMA) from aqueous solution on silicon substrates. The investigated polyampholyte is characterized by a small molecular weight around 15,000 g/mol and a big positively charged PDMAEMA block. The adsorbed amount determined by ellipsometry was str ongly influenced by the pH of the adsorption solution. Using dynamic light scattering polyampholytic structures with diameters around 50 nm were found in aqueous solution. The hydrodynamic diameter was hardly affected by changing the pH of the polymer solution. Analogous regular structures were also found by scanning force microscopy (SFM) and grazing incidence, small angle X-ray scattering (GISAXS) at the silicon surface after the adsorption process. While SFM provides a topographical image of a small part of the adsorbed polyampholytic layer; GISAXS was used to get a statistical description of the lateral surface structures. The adsorbed structures were highly regular and their sizes were nearly pH independent over a lar ge pH region. Only directly at the isoelectric point of the polyampholyte larger adsorbed structures were observed. Compared with earlier investigated PMAA-b-PDMAEMA systems we are now able to prepare highly regular polyampholytic structures at silicon surfaces. There are two kinds of interactions for the adsorbed micelles. First, the charged block of the chains is directly attracted to the substrate via electrostatic interactions, while the uncharged part of the chains is only hydrophobically attracted via the hydrophobic core of the adsorbed micelle.

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Section: Scanning Force Microscopymentioning

confidence: 99%

Highly Regular Polyampholytic Structures Adsorbed Directly from Solution

Mahltig

Müller‐Buschbaum

Wolkenhauer

et al. 2001

Journal of Colloid and Interface Science

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“…However, with decreasing scattering volume like in the thin-film geometry the transmission geometry is no longer applicable. Recently, the technique of grazing incidence small-angle X-ray scattering (GISAXS) was successfully applied to soft condensed matter samples in the thin-film geometry [11,12,13,14,15]. The transmission geometry is replaced by a reflection one.…”

Section: Introductionmentioning

confidence: 99%

“…This yields a surface sensitivity, which enables the investigation of surfaces and thin films with thicknesses down to the sub-monomolecular range, thus becoming sensitive to nanostructures. Following the same principles as in the transmission geometry, larger length scales are addressable by an increase in the sample detector distance [13].…”

Section: Introductionmentioning

confidence: 99%

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

2003

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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.

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“…Our aim is to probe lateral length scales ranging from a few nanometres up to hundreds of nanometres [1,2] of colloidal systems with a defined mean particle dimension and typical polydispersities with standard deviations σ = 0−0.6, which is often sufficient to understand material film properties [3]. Polydisperse particles can be a e-mail: gutmann@mpip-mainz.mpg.de located as islands at the film/air interface or buried within a thin film matrix.…”

Section: Introductionmentioning

confidence: 99%

Global scattering functions: a tool for grazing incidence small angle X-ray scattering (GISAXS) data analysis of low correlated lateral structures

Lenz

Bonini

Nett

et al. 2010

Eur. Phys. J. Appl. Phys.

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Abstract. In this article we discuss the applicability of global scattering functions for structure analysis of Grazing Incidence Small Angle X-ray Scattering (GISAXS) data. Contrary to rigorous analysis of the full 2-D detector image, which can be performed with complex simulation models, the global scattering functions described here will be used to model transverse detector scans in the q reciprocal scattering planes. In contrast to a full GISAXS analysis, this procedure cannot explain structural features perpendicular to the sample plane. The discussed method is useful for the analysis of weakly correlated films. These films are e.g. found in polymer inorganic composite materials based on commercially available nanoparticles. In hybrid material systems polydisperse structures, including particle aggregates without precisely defined shape are formed. The pictured approach, which models scattering in terms of structural levels, has been previously applied with success in conventional transmission SAXS geometry. It is based on conventional exponential and power laws. Hence, data analysis becomes less complex compared to simulation approaches. Here we examine if this unified fitting model can be used to model diffuse, non specular scattering resulting from GISAXS. In this context the applicability and limit of its application to diffuse scattering in the GISAXS geometry is discussed. Furthermore diffuse q scattering from different ideal particle types is simulated and compared with fitted results. To verify our approach, fit results from experimental GISAXS curves obtained for real samples are compared with results from Scanning Probe Microscopy and Scanning Electron Microscopy studies. The samples investigated range from evaporated Au films to hybrid TiO2/polymer films and demonstrate the usefulness in the structural analysis of complex films.

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Determination of micrometer length scales with an X-ray reflection ultra small-angle scattering set-up

Cited by 41 publications

References 17 publications

Highly Regular Polyampholytic Structures Adsorbed Directly from Solution

Highly Regular Polyampholytic Structures Adsorbed Directly from Solution

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

Global scattering functions: a tool for grazing incidence small angle X-ray scattering (GISAXS) data analysis of low correlated lateral structures

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