Small-angle options of the upgraded ultrasmall-angle x-ray scattering beamline BW4 at HASYLAB

Roth, Stephan V.; Döhrmann, Ralph; Dommach, M.; Kuhlmann, Marion; Kröger, Ingo; Gehrke, Rainer; Walter, H.; Schroer, Christian G.; Lengeler, B.; Müller‐Buschbaum, Peter

doi:10.1063/1.2336195

Cited by 165 publications

(158 citation statements)

References 38 publications

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“…30 In particular, when the scattered beam is collected in a small angle ͑GISAXS͒ or ultrasmall angle configuration it enables the characterization of surface order on large or very large scales: for example, structures up to 20 m can be detected at state of the art beamlines. 31 Using focusing optics, available at these beamlines, 32 the high reciprocal space resolution can be coupled to a certain extent with a real-space resolution in the 1 -50 m range, thus allowing to perform a scanning analysis of the samples.…”

Section: Introductionmentioning

confidence: 99%

Flow at interfaces: A new device for x-ray surface scattering investigations

Moulin

Roth²,

Müller‐Buschbaum

2008

Review of Scientific Instruments

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A fluidic cell based setup is described which allows for microbeam grazing incidence small angle x-ray scattering characterization of the interface between a solid substrate and a flowing liquid. This cell can potentially be used to study in situ a wide variety of systems ranging from synthetic and natural colloids to biological molecules. The selected channel geometry enables the characterization of the solid-liquid interface during mixing of different solutions. As a proof of concept, measurements on an aqueous gold nanoparticle solution in contact with a glass surface are presented that show that the structure at the interface can be probed during flow.

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Section: Introductionmentioning

confidence: 99%

Flow at interfaces: A new device for x-ray surface scattering investigations

Moulin

Roth²,

Müller‐Buschbaum

2008

Review of Scientific Instruments

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“…GISAXS experiments were performed at HASYLAB beamline BW4 equipped with a MarCCD camera as an area detector [21]. The wavelength was 1.388 Å and the sample-todetector distance 2.23 m. The beam was focused by Beryllium compound refractive lenses to a size of $40 lm Â 20 lm (horizontal Â vertical) at the sample position.…”

Section: Methodsmentioning

confidence: 99%

Creation of lateral structures in diblock copolymer thin films during vapor uptake and subsequent drying – Effect of film thickness

Sepe

Černoch

Štěpánek

et al. 2014

European Polymer Journal

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a b s t r a c tWe have studied the structure formation in compositionally nearly symmetric poly(4-octylstyrene-b-butylmethacrylate) diblock copolymer films during exposure to saturated vapor of n-hexane (a poor solvent for both blocks) and subsequent drying using real-time, in situ grazing-incidence small-angle X-ray scattering (GISAXS). Previous bulk studies revealed a lamellar structure after thermo-annealing; and surface studies on hexane treated samples revealed a lateral surface structure (Č ernoch et al., 2007) [14]. We focus here on the effect of film thickness which is varied between 1.3 and 2.0 times the bulk lamellar thickness. We report on the lateral repeat distance as well as on the correlation length in the film plane. Complex, non-monotonous behavior is observed for both parameters. Upon drying, the lateral structure created during vapor treatment is stable only for the thick film, not for the intermediate and the thin film. The kinetics depends strongly on the film thickness; especially for the thinnest film, it is very slow. For all film thicknesses, we attempt to identify the most stable morphology, occurring when the inner film structure is close to the one in the bulk.

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“…The grazing incidence small angle X-ray scattering (GISAXS [23] ) experiments were performed at the beamline BW4 [24] of the DORIS III storage ring at HASYLAB (DESY, Hamburg). Sketch of the GISAXS geometry is shown in Figure 2.…”

Section: Methodsmentioning

confidence: 99%

Stripe‐Like Pattern Formation in Airbrush‐Spray Deposition of Colloidal Polymer Film

et al. 2010

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Thin films and multilayer structures are used in a wide range of applications. To name just a few: sensor coating, [1][2][3] microelectronics, [4] solar cell technology, [5,6] and magnetic recording. [7] In the last few years, organic-based hybrid devices received strong attention from both academy and industry because of their potential for low-cost production and flexible device applications. [5] In order to improve the device performances, new approaches are needed to install thin films showing lateral order and high uniformity over large areas. Many methods have already been developed: bottom-up approaches such as solution casting, [8] spincoating, [5] inkjet printing, [9,10] dip-coating, [11] and also topdown approaches such as lithography [12,13] or vacuum deposition. [14] Recently, the novel technique of airbrush-spray deposition was used in the fabrication of organic-based multilayer devices such as diodes, [15] transistors, [16] semiconductors, [17] electrolyte films, [18,19] and solar cells. [20][21][22] The airbrush-spray coating technique allows performing fast and economic deposition of organic-based layers showing high structural uniformity over large areas and is thus of great interest in industrial applications. ExperimentalFor the polymer coating, we used a commercial airbrush-spray (Harder & Steenbeck, Evolution Silverline) with a needle diameter of 30 mm (see Fig. 1). Two different types of aqueous colloidal suspensions (provided by Kisker GbR, Steinfurt, Germany) were deposited: polystyrene (PS) colloids (initial concentration: 2.5 wt%) and carboxylated polystyrene (cPS) colloids (initial concentration: 5.0 wt%). Both types of colloids have a nominal diameter of 96 nm. Two different solvents were used for further dilution, namely deionized water and ethanol. Influence of the solvent on the film lateral ordering will be discussed later. Spray coatings were performed on flat Silicon (Si) substrates (18 Â 30 mm 2 ) at an air pressure P ¼ 3 bar in a horizontal configuration. Prior to use, the Si wafers were cleaned in a basic bath (35 mL of 25% ammoniac, 25 mL of 35% hydrogen peroxide, and 350 mL of deionized water) at a temperature of 75 8C. The cleaned substrates were further individually rinsed in deionized water and dried using nitrogen flow.Two different spray-deposition modes were examined. In the first mode, the coating is performed in one single cycle at a short spray nozzle-to-substrate distance (D SS ¼ 73 mm). In the second mode, the coating consists in three spray cycles at a larger spray nozzle-to-substrate distance (D SS ¼ 142 mm). These two distances ensure a complete coating of the substrate. By enlarging the distance, one can reduce the amount of solvent (by evaporation) impinging on the substrate. A spray cycle is 1 s, the time between two successive spray cycles (second coating mode) 5 s. The total coating time is 1 s in the first mode and 3 s in the second mode. An overview of the parameter sets used in this study is given in We use the versatile technique of Grazing incidence ...

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Small-angle options of the upgraded ultrasmall-angle x-ray scattering beamline BW4 at HASYLAB

Cited by 165 publications

References 38 publications

Flow at interfaces: A new device for x-ray surface scattering investigations

Flow at interfaces: A new device for x-ray surface scattering investigations

Creation of lateral structures in diblock copolymer thin films during vapor uptake and subsequent drying – Effect of film thickness

Stripe‐Like Pattern Formation in Airbrush‐Spray Deposition of Colloidal Polymer Film

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