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For advanced functional polymers such as biopolymers, biomimic polymers, brush polymers, star polymers, dendritic polymers, and block copolymers, information about their surface structures, morphologies, and atomic structures is essential for understanding their properties and investigating their potential applications. Grazing incidence X-ray scattering (GIXS) is established for the last 15 years as the most powerful, versatile, and nondestructive tool for determining these structural details when performed with the aid of an advanced third-generation synchrotron radiation source with high flux, high energy resolution, energy tunability, and small beam size. One particular merit of this technique is that GIXS data can be obtained facilely for material specimens of any size, type, or shape. However, GIXS data analysis requires an understanding of GIXS theory and of refraction and reflection effects, and for any given material specimen, the best methods for extracting the form factor and the structure factor from the data need to be established. GIXS theory is reviewed here from the perspective of practical GIXS measurements and quantitative data analysis. In addition, schemes are discussed for the detailed analysis of GIXS data for the various self-assembled nanostructures of functional homopolymers, brush, star, and dendritic polymers, and block copolymers. Moreover, enhancements to the GIXS technique are discussed that can significantly improve its structure analysis by using the new synchrotron radiation sources such as third-generation X-ray sources with picosecond pulses and partial coherence and fourth-generation X-ray laser sources with femtosecond pulses and full coherence.
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http://dx.doi.org/10.1002/marc.201400025 | DOI Listing |
ACS Nano
January 2025
Fritz Haber Institute of the Max Planck Society, Berlin D-14195, Germany.
Functionalization and volatilization are competing reactions during the oxidation of carbonaceous materials and are important processes in many different areas of science and technology. Here, we present a combined ambient pressure X-ray photoelectron spectroscopy (APXPS) and grazing incidence X-ray scattering (GIXS) investigation of the oxidation of oleic acid ligands surrounding NaYF nanoparticles (NPs) deposited onto SiO/Si substrates. While APXPS monitors the evolution of the oxidation products, GIXS provides insight into the morphology of the ligands and particles before and after the oxidation.
View Article and Find Full Text PDFLangmuir
January 2022
Cavendish Laboratory, Department of Physics, University of Cambridge, J. J. Thomson Avenue, Cambridge CB3 0HE, United Kingdom.
In this feature article, we discuss the fundamental use of materials-characterization methods that determine structural information on the dye···TiO interface in dye-sensitized solar cells (DSCs). This interface is usually buried within the DSC and submerged in solvent and electrolyte, which renders such metrological work nontrivial. We will show how - X-ray reflectometry (XRR), atomic-force microscopy (AFM), grazing-incidence X-ray scattering (GIXS), pair-distribution-function analysis of X-ray diffraction data (gaPDF), and - neutron reflectometry (NR) can be used to deliver specific structural information on the dye···TiO interface regarding dye anchoring, dye aggregation, molecular dye orientation, intermolecular spacing between dye molecules, interactions between the dye molecules and the TiO surface, and interactions between the dye molecules and the electrolyte components and precursors.
View Article and Find Full Text PDFSci Rep
February 2015
Center for Advanced Radiation Sources, The University of Chicago, Chicago, IL 60637, USA.
We report on the counter intuitive reversible crystallisation of two-dimensional monolayer of Trisilanolisobutyl Polyhedral Oligomeric SilSesquioxane (TBPOSS) on water surface using synchrotron x-ray scattering measurements. Amphiphilic TBPOSS form rugged monolayers and Grazing Incidence X-ray Scattering (GIXS) measurements reveal that the in-plane inter-particle correlation peaks, characteristic of two-dimensional system, observed before transition is replaced by intense localized spots after transition. The measured x-ray scattering data of the non-equilibrium crystalline phase on the air-water interface could be explained with a model that assumes periodic stacking of the TBPOSS dimers.
View Article and Find Full Text PDFMacromol Rapid Commun
May 2014
Department of Chemistry, Division of Advanced Materials Science, Pohang Accelerator Laboratory, Center for Electro-Photo Behaviors in Advanced Molecular Systems, Polymer Research Institute, and BK School of Molecular Science, Pohang University of Science & Technology, Pohang, 790-784, Republic of Ko