Comparing the backfilling of mesoporous titania thin films with hole conductors of different sizes sharing the same mass density

Märkl, Raphael S.; Hohn, Nuri; Hupf, Emanuel; Bießmann, Lorenz; Körstgens, Volker; Kreuzer, Lucas P.; Mangiapia, Gaetano; Pomm, Matthias; Kriele, Armin; Rivard, Eric; Müller‐Buschbaum, Peter

doi:10.1107/s2052252520000913

Cited by 2 publications

(1 citation statement)

References 52 publications

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“…Neutrons are also uniquely sensitive to hydrogen and its isotope, deuterium. , With suitable instrumentation, GISANS has been increasingly used over the past three decades . Müler-Buschbaum pioneered the earliest studies on thin films by GISANS in an extensive series of studies on polymer thin films about surface roughness, interdiffusion of polymers, single-chain conformations, , dewetting of homopolymers and copolymers, − hydration of micelles, adhesive-adherent interfaces, and composite materials for photovoltaic, − magnetic, , and Li-ion battery applications. , Felcher and Adenwalla investigated Zeeman splitting when polarized neutrons impinged on a ferromagnetic surface at a grazing angle . GISANS has since been widely used to study micelles − and other nanomaterials near surfaces and interfaces .…”

Section: Introductionmentioning

confidence: 99%

Using Grazing-Incidence Small-Angle Neutron Scattering to Study the Orientation of Block Copolymer Morphologies in Thin Films

Heller

et al. 2023

Macromolecules

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We used grazing-incidence small-angle neutron scattering (GISANS) to probe the depth-dependent orientation of self-assembled morphologies of block copolymers. A hydrophobic−hydrophobic block copolymer, poly(solketal methacrylate)-blockpolystyrene (PSM-b-PS), was synthesized and spin-coated into films tens of nanometers in thickness where the polymers adopted a disordered state. PSM-b-PS was then hydrolyzed by exposing the polymer thin film to trifluoroacetic acid vapor or embedding a photoacid generator in the film during spin coating, followed by exposure to UV light. The hydrolysis converted the block copolymer into a hydrophilic−hydrophobic block copolymer, poly(glycerol monomethacrylate)-block-polystyrene (PGM-b-PS), significantly increasing the segmental interaction parameter (χ) and causing microphase separation of the copolymers. GISANS was used to study the depth-dependent structure of the films and revealed that the orientation of the microphase-separated structure differed at the polymer−air and polymer−substrate interfaces. In the regions where the lamellae were parallel to the interfaces, the orientation propagated into the film from the interfaces. However, in the areas where the lamellae were perpendicular to the interfaces, the orientation did not persist with increasing distance from the interfaces.

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Section: Introductionmentioning

confidence: 99%

Using Grazing-Incidence Small-Angle Neutron Scattering to Study the Orientation of Block Copolymer Morphologies in Thin Films

Heller

et al. 2023

Macromolecules

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3D printed spherical environmental chamber for neutron reflectometry and grazing-incidence small-angle neutron scattering experiments

Widmann

Kreuzer

Mangiapia

et al. 2020

Review of Scientific Instruments

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In neutron scattering on soft matter, an important concern is the control and stability of environmental conditions surrounding the sample. Complex sample environment setups are often expensive to fabricate or simply not achievable by conventional workshop manufacturing. We make use of state-of-the-art 3D metal-printing technology to realize a sample environment for large sample sizes, optimized for investigations on thin film samples with neutron reflectometry (NR) and grazing-incidence small-angle neutron scattering (GISANS). With the flexibility and freedom of design given by 3D metal-printing, a spherical chamber with fluidic channels inside its walls is printed from an AlSi10Mg powder via selective laser melting (SLM). The thin channels ensure a homogeneous heating of the sample environment from all directions and allow for quick temperature switches in well-equilibrated atmospheres. In order to optimize the channel layout, flow simulations were carried out and verified in temperature switching tests. The spherical, edgeless design aids the prevention of condensation inside the chamber in case of high humidity conditions. The large volume of the sample chamber allows for high flexibility in sample size and geometry. While a small-angle neutron scattering (SANS) measurement through the chamber walls reveals a strong isotropic scattering signal resulting from the evenly orientated granular structure introduced by SLM, a second SANS measurement through the windows shows no additional background originating from the chamber. Exemplary GISANS and NR measurements in time-of-flight mode are shown to prove that the chamber provides a stable, background free sample environment for the investigation of thin films.

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Comparing the backfilling of mesoporous titania thin films with hole conductors of different sizes sharing the same mass density

Cited by 2 publications

References 52 publications

Using Grazing-Incidence Small-Angle Neutron Scattering to Study the Orientation of Block Copolymer Morphologies in Thin Films

Using Grazing-Incidence Small-Angle Neutron Scattering to Study the Orientation of Block Copolymer Morphologies in Thin Films

3D printed spherical environmental chamber for neutron reflectometry and grazing-incidence small-angle neutron scattering experiments

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