X-ray scattering is a structural characterization tool that has impacted diverse fields of study. It is unique in its ability to examine materials in real time and under realistic sample environments, enabling researchers to understand morphology at nanometer and angstrom length scales using complementary small and wide angle X-ray scattering (SAXS, WAXS), respectively. Herein, we focus on the use of SAXS to examine nanoscale particulate systems. We provide a theoretical foundation for X-ray scattering, considering both form factor and structure factor, as well as the use of correlation functions, which may be used to determine a particle’s size, size distribution, shape, and organization into hierarchical structures. The theory is expanded upon with contemporary use cases. Both transmission and reflection (grazing incidence) geometries are addressed, as well as the combination of SAXS with other X-ray and non-X-ray characterization tools. We conclude with an examination of several key areas of research w...

Small Angle X-ray Scattering for Nanoparticle Research

The electrochemical carbon dioxide reduction reaction (CO2RR) to simultaneously produce carbon monoxide (CO) and hydrogen (H2) has been achieved on carbon supported palladium (Pd/C) nanoparticles in an aqueous electrolyte. The synthesis gas product has a CO to H2 ratio between 0.5 and 1, which is in the desirable range for thermochemical synthesis of methanol and Fischer–Tropsch reactions using existing industrial processes. In situ X-ray absorption spectroscopy in both near-edge (XANES) and extended regions (EXAFS) and in situ X-ray diffraction show that Pd has transformed into β-phase palladium hydride (β-PdH) during the CO2RR. Density functional theory (DFT) calculations demonstrate that the binding energies of both adsorbed CO and H are significantly weakened on PdH than on Pd surfaces, and that these energies are potential descriptors to facilitate the search for more efficient electrocatalysts for syngas production through the CO2RR.

Electrochemical reduction of CO2 to synthesis gas with controlled CO/H2 ratios

This review focuses on important stability issues facing amine-functionalized CO2 adsorbents, including amine-grafted and amine-impregnated silicas, zeolites, metal–organic frameworks and carbons. During the past couple of decades, major advances were achieved in understanding and improving the performance of such materials, particularly in terms of CO2 adsorptive properties such as adsorption capacity, selectivity and kinetics. Nonetheless, to pave the way toward commercialization of adsorption-based CO2 capture technologies, in addition to other attributes, adsorbent materials should be stable over many thousands of adsorption–desorption cycles. Adsorbent stability, which is of utmost importance as it determines adsorbent lifetime and operational costs of CO2 capture, is a multifaceted issue involving thermal, hydrothermal, and chemical stability. Here we discuss the impact of the adsorbent physical and chemical properties, the feed gas composition and characteristics, and the adsorption–desorption operational parameters on the long-term stability of amine-functionalized CO2 adsorbents. We also review important insights associated with the underlying deactivation pathways of the adsorbents upon exposure to high temperature, oxygen, dry CO2, sulfur-containing compounds, nitrogen oxides, oxygen and steam. Finally, specific recommendations are provided to address outstanding stability issues.

Stability of amine-functionalized CO2 adsorbents: a multifaceted puzzle.

https://cyberleninka.org/article/n/1459363.pdf

Solid amine sorbents for CO2 capture by chemical adsorption: A review

Nanoparticles have drawn significant attention in biomedicine due to their unique optical, thermal, magnetic and electrical properties which are highly related to their size and morphologies. Recently, microfluidic systems have shown promising potential to modulate critical stages in nanosynthesis, such as nucleation, growth and reaction conditions so that the size, size distribution, morphology, and reproducibility of nanoparticles are optimized in a high throughput manner. In this review, we put an emphasis on a decade of developments of microfluidic systems for engineering nanoparticles in various applications including imaging, biosensing, drug delivery, and theranostic applications.

Controllable synthesis of functional nanoparticles by microfluidic platforms for biomedical applications - a review.

Molecular basket sorbents polyethylenimine–SBA-15 for CO2 capture from flue gas: Characterization and sorption properties

A novel microfluidic reactor for in situ small-angle X-ray scattering (SAXS) and X-ray absorption fine structure spectroscopy (XAFS) of Pd colloidal nanoparticles synthesis is reported. The microreactor allows time resolution ranging from milliseconds to several minutes with a residence time of over an hour. The synthesis of colloidal Pd nanoparticles is investigated in the presence of oleylamine and trioctylphosphine ligands. For both ligands, SAXS results show the synthesis proceeds through slow, continuous nucleation as evidenced by a continuous increase in the number of particles. Growth is autocatalytic and fast at the early times; then, despite the availability of a large percentage of unreacted Pd precursor, growth slows dramatically and the Pd nanoparticle diameter reaches a plateau while more nanoparticles continue to form. In situ XAFS reveals an increase in Pd–P coordination coinciding with the time of slowed growth. The combined SAXS and XAFS results strongly suggest that the capping ligands p...

Synthesis of 1 nm Pd Nanoparticles in a Microfluidic Reactor: Insights from in Situ X ray Absorption Fine Structure Spectroscopy and Small-Angle X ray Scattering

Synthesis of 1nm Pd Nanoparticles in a Microfluidic Reactor: Insights from In Situ XAFS and SAXS

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Molecular basket sorbents polyethylenimine–SBA-15 for CO2 capture from flue gas: Characterization and sorption properties

Synthesis of 1 nm Pd Nanoparticles in a Microfluidic Reactor: Insights from in Situ X ray Absorption Fine Structure Spectroscopy and Small-Angle X ray Scattering

Synthesis of 1nm Pd Nanoparticles in a Microfluidic Reactor: Insights from In Situ XAFS and SAXS