Solid state nuclear magnetic resonance (ssNMR) is a powerful and attractive characterization method for obtaining insights into the chemical structure and dynamics of a wide range of materials. Current interest in cellulose-based materials, as sustainable and renewable natural polymer products, requires deep investigation and analysis of the chemical structure, molecular packing, end chain motion, functional modification, and solvent–matrix interactions, which strongly dictate the final product properties and tailor their end applications. In comparison to other spectroscopic techniques, on an atomic level, ssNMR is considered more advanced, especially in the structural analysis of cellulose-based materials; however, due to a dearth in the availability of a broad range of pulse sequences, and time consuming experiments, its capabilities are underestimated. This critical review article presents the comprehensive and up-to-date work done using ssNMR, including the most advanced NMR strategies used to overcome and resolve the structural difficulties present in different types of cellulose-based materials.
Upconversion nanoparticles (UCNPs) and carbon quantum dots (CQDs) have recently received a lot of attention as promising materials to improve the stability and efficiency of perovskite solar cells (PSCs). This is because they can passivate the surfaces of perovskite-sensitive materials and act as a spectrum converter for sunlight. In this study, we mixed and added both promising nanomaterials to PSC layers at the ideal mixing ratios. When compared to the pristine PSCs, the fabricated PSCs showed improved power conversion efficiency (PCE), from 16.57% to 20.44%, a higher photocurrent, and a superior fill factor (FF), which increased from 70% to 75%. Furthermore, the incorporation of CQDs into the manufactured PSCs shielded the perovskite layer from water contact, producing a device that was more stable than the original.
Production of renewable and modified starch-based products was achieved using a sustainable catalyst and an environmentally friendly drying process via supercritical CO 2 . Potato starch was modified via a sustainable and green esterification process with acetic anhydride reagent implementing a novel organocatalytic pathway at different periods of time (0.5, 3 and 7 h) by applying an esterification reaction at 120 C targeting intermediate degrees of substitution (i.e., 0.2 < DS <1.5) finding potential applications as polymer packaging materials. The final modified samples were divided into two fractions, where the first fraction was dried under vacuum at 80 C for 24 h and the second fraction was dried under supercritical CO 2 at 40 C and 100 bars for 2 h. The final products were analyzed using an array of characterization techniques such as Fourier transform infrared (FTIR), Proton nuclear magnetic resonance ( 1 H-NMR), scanning electron microscopy (SEM), X-ray diffraction (XRD), N 2 physisorption, thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), and Karl Fischer. The chemical structure of both fractions was similar as confirmed by the different characterization techniques. Drying under supercritical CO 2 preserved some pores in the modified starch materials as opposed to thermal oven drying, as was confirmed by N 2 physisorption measurements. The degree of substitution (DS) was determined using three different techniques; titration, high performance liquid chromatography (HPLC) and solution state proton nuclear magnetic resonance ( 1 H NMR) spectroscopy and the values were greater than 0.2 and less than 1.5 indicating intermediate degrees of substitution.
Solid-state NMR is a nondestructive and noninvasive technique used to study the chemical structure and dynamics of starch-based materials and to bridge the gap between structure–function relationships and industrial applications. The study of crystallinity, chemical modification, product blending, molecular packing, amylose–amylopectin ratio, end chain motion, and solvent–matrix interactions is essential for tailoring starch product properties to various applications. This article aims to provide a comprehensive and critical review of research characterizing starch-based materials using solid-state NMR, and to briefly introduce the most advanced and promising NMR strategies and hardware designs used to overcome the sensitivity and resolution issues involved in structure–function relationships.
Zeolites are crystalline metallosilicates displaying unique physicochemical properties with widespread applications in catalysis, adsorption, and separation. They are generally obtained by a multi-step process that starts with primary mixture aging, followed by hydrothermal crystallization, washing, drying, and, finally, a calcination step. However, the zeolites obtained are in the powder form and because of generating a pressure drop in industrial fixed bed reactors, not applicable for industrial purposes. To overcome such drawbacks, zeolites are shaped into appropriate geometries and the desired size (a few centimeters) using extrusion, where zeolite powders are mixed with binders (e.g., mineral clays or inorganic oxides). The presence of binders provides good mechanical strength against crushing in shaped zeolites, but binders may have adverse impacts on zeolite catalytic and sorption properties, such as active site dilution and pore blockage. The latter is more pronounced when the binder has a smaller particle size, which makes the zeolite internal active sites mainly inaccessible. In addition to the shaping requirements, a hierarchical structure with different levels of porosity (micro-, meso-, and macropores) and an interconnected network are essential to decrease the diffusion limitation inside the zeolite micropores as well as to increase the mass transfer through the presence of larger auxiliary pores. Thus, the generation of hierarchical structure and its preservation during the shaping step is of great importance. The aim of this review is to provide a comprehensive survey and detailed overview on the binder-containing extrusion technique compared to alternative shaping technologies with improved mass transfer properties. An emphasis is allocated to those techniques that have been less discussed in detail in the literature.
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