Wide-angle X-ray Diffraction Research Articles

An efficient β-nucleating agent with high lattice matching rate for plate-like crystallization of polypropylene random copolymer.

It is challenging to naturally produce large amounts of β-crystals by directly adding a commercial β-nucleating agent (β-NA) into polypropylene random copolymer (PPR) at present. In this work, a novel rare earth β-NA WBN-28 was directly introduced into PPR to prepare β-PPR with high β-crystal conversion. The results of differential scanning calorimetry (DSC) and wide-angle X-ray diffraction (WAXD) indicated that it is an efficient β-NA for PPR. The β-conversion rate (β-CR) could surpass 85% when the nucleating agent content was mere 0.05%. With the further increment of nucleating agent, the β-CR increased gradually, which could reach 89.5% and 86.9% respectively calculated by DSC and WAXD when the addition amount was 0.4%. The incredible high β-CR delayed the βα-recrystallization in isothermal crystallization. The fusion peak of α-crystal was unobserved below the isothermal crystallization temperature of 122 °C when the addition amount was more than 0.2%. Furthermore, there was a highly ordered structure in WBN-28 with the periodicity of 12.89 Å, which was approximately twice of the unit cell parameter in the c direction of β-PP, indicating a high lattice matching rate between them. Intuitively observed by polarizing optical microscope (POM), the crystal grains of the blends with β-NA were more refined and finally crystallized in a plate-like shape. The forming process of the plate-like β crystalline regions were proposed by scanning electron microscope (SEM) and POM.

Thermal transformation of date seeds from nonporous to porous materials: Insights on structural changes using chemical and physical characterization

The comprehension of the structure and morphology of carbonized bio-based materials remains incomplete. Diverse biomaterials have been employed in the carbonization process to create porous materials for various environmental remediation applications, such as air filtration and water treatment. This study explores the impact of pyrolysis temperature on the chemical structure, porosity, and morphology of date seeds. Molecular-level changes in the carbonized date seeds were investigated using time-of-flight secondary ion mass spectrometry (ToF-SIMS) and X-ray photoelectron spectroscopy (XPS). Wide angle X-ray diffraction (WXRD) illustrated the transition from semi-crystalline to amorphous material. Concurrently, scanning electron microscopy (SEM) and Brunauer–Emmett–Teller (BET) surface area analyses were employed to monitor the alterations in morphology and porosity. The amorphous pyrolyzed date seeds displayed a BET surface area of 117 ± 13 m2 g−1. These findings contribute valuable insights into the structural transformations of date seed chemistry during the carbonization process.

Wood fibre alkalization effect on the thermal stability of meranti wood flour: a modification of the conventional method

Alkalization of plant or wood fibre (WF) is the most widely used method of chemical modification to improve reinforcement in thermoplastic composites. This process involves the complete or partial removal of extractives and or modification of lignocellulosic material. While research has shown that removal of the less thermally stable extractives results in an improvement in fibre thermal stability, in the current work it has been shown through single-factor analyses, Fourier transform infrared microscopy, scanning electron microscopy, thermogravimetric analyses and wide angle X-ray diffraction that meranti WF thermal stability is largely influenced by the holistic changes in the WF structure, which itself is affected by alkalization factors. After implementing stepwise regression on a central composite design, no empirical model could be established to explain or predict thermal stability due to interaction of treatment factors. As a result, single-factor analyses of temperature, time and alkali concentration were conducted. Single-factor analyses showed that different combinations of time, temperature and alkali concentration through a central composite design result in WF with different thermal stabilities, lignocellulosic content, crystallinities, crystallite sizes, extractives content and morphology. Alkali-treated meranti WF showed lower thermal stability compared to the untreated WF. Mild treatment conditions (e.g. 50 °C/30 min/5%) were seen to result in the most thermally stable WF. Increasing temperature, treatment duration and alkali concentration increased thermal stabilities except at harsh conditions (e.g. 50 °C/90 min/15%). A combination of high alkali concentration and long treatment times showed a combined detrimental effect on WF thermal stability. Changes in the lignocellulosic structure, crystallinity, crystallite sizes and surface features explain the observed changes in thermal stabilities.

Multiscale study of the chiral self-assembly of cellulose nanocrystals during the frontal ultrafiltration process.

The structural organization of cellulose nanocrystal (CNC) suspensions at the membrane surface during frontal ultrafiltration has been characterized, for the first time, at the nano- and microscale by in situ small-angle X-ray and light scattering (SAXS and SALS, respectively). During filtration, the particles assembled at the membrane surface and formed the so-called concentration polarization layer (CPL), which contains CNCs arranged in a chiral nematic (cholesteric) helicoidal structure, with the long axis of the CNCs oriented parallel to the membrane surface, and the helical axis of the cholesteric structure oriented perpendicular to the membrane surface. The self-organization of CNCs in the form of oriented cholesteric structures was further characterized by a pitch gradient in the CPL. The structure of the CPL was also investigated upon release of the transmembrane pressure. SAXS data revealed a relaxation process associated with a diffusion of the CNCs from the membrane surface towards the bulk, while SALS measurements revealed a re-organization of the cholesteric phase that was preserved all along the deposit. The preservation of the observed structure after 14 days of continuous filtration followed by air-drying was confirmed using scanning electron microscopy and wide-angle X-ray diffraction, demonstrating the feasibility of the process scale-up.

Physiochemical and functional properties of Moringa oleifera protein obtained by isoelectric precipitation

The work investigated the effect of extraction pH (10 or 11) and precipitation pH (4 or 4.5) on the physicochemical and functional properties of Moringa oleifera protein. The physicochemical characteristics of Moringa leaf powder were analyzed using proximate quantification based on AOAC standard methods. The thermal, spectral, x-ray diffraction data were collected using the differential scanning calorimetric, Fourier transform infrared spectroscopy (FTIR), and wide-angle x-ray diffraction. The extraction at pH 10 and the precipitation process at pH 4.5 generated the highest protein content of 58.88%. Some of the functional properties of this pH combination were emulsion activity at 29.67%, emulsion stability at 50.45%, protein solubility at 32.36%, and water absorption capacity of 4.78 mL water/g. The thermal properties suggested the denaturation temperature of Moringa protein powder at 75°C, which was comparable to that previously reported plantbased protein isolate. FTIR and x-ray spectra argued the domination of amorphous protein fraction with a trace of lipid and carbohydrate. With these characteristics, protein has great potential to be used for food and drug applications.

Alternating vs. random amphiphilic polydisulfides: aggregation, enzyme activity inhibition and redox-responsive guest release.

Herein, we report the synthesis of an alternating copolymer (ACP) with a bio-reducible amphiphilic polydisulfide backbone and highlight the impact of the alternating monomer connectivity on the self-assembly, morphology, chain-exchange dynamics, drug-release kinetics, and enzyme activity inhibition. Condensation polymerization between hydrophobic 1,10-bis(pyridin-2-yldisulfaneyl)decane and hydrophilic 2,3-mercaptosuccinic acid (1.04 : 1.00 ratio) generated amphiphilic ACP P1 (Mw = 8450 g mol-1, Đ = 1.3), which exhibited self-assembly in water, leading to the formation of an ultra-thin (height <5.0 nm) entangled fibrillar network. In contrast, structurally similar amphiphilic random copolymer P2 exhibited a truncated irregular disc-like morphology under the same conditions. It is postulated that due to the perfect alternating sequence of the hydrophobic and hydrophilic segments in P1, its immiscibility-driven aggregation in water leads to a pleated structure, which further assembles and forms the observed long fibrillar structures, similar to crystallization-driven self-assembly. In fact, wide-angle X-ray diffraction (WXRD) analysis of a lyophilized P1 sample showed sharp peaks, indicating its crystalline nature (approximately 37% crystallinity), and these were completely missing for P2. The effect of such distinct self-assembly on the chain-exchange dynamics was probed by fluorescence resonance energy transfer (FRET) using 3,3'-dioctadecyloxacarbocyanine perchlorate (DiO) and 1,1'-dioctadecyl-3,3,3',3'-tetramethylindocarbocyanine perchlorate (DiI) as the FRET-donor and -acceptor, respectively. For DiI- and DiO-entrapped solutions of P1, when mixed, no prominent FRET appeared even after 24 h. In sharp contrast, for P2, intense FRET emission occurred, and the FRET ratio (approximately 0.9) reached saturation in approximately 15 h, indicating the greatly enhanced kinetic stability of P1 aggregates. Glutathione-induced release of encapsulated Nile red showed much slower kinetics for P1 compared to that of P2, which was corroborated by the observed slow chain-exchange dynamics of the highly stable alternating copolymer assembly. Furthermore, the well-ordered assembly of P1 exhibited an excellent surface-functional group display (zeta potential of -32 mV compared to -14 mV for P2), which resulted in the effective recognition of the α-chymotrypsin (Cht) protein surface by electrostatic interaction. Consequently, P1 significantly (>70%) suppressed the enzymatic activity of Cht, while in the presence of P2, the enzyme was still active with >70% efficacy.

Macromolecular structure development of dry-spinning UHMWPE fibers through the industrial high-ratio hot-drawing process

Ultra-high molecular weight polyethylene (UHMWPE) and its decalin suspension were subjected to several industrial processes including swelling, dissolving, spinning, drying, and multi-stage high-ratio hot drawing to fabricate UHMWPE fibers (UPE fibers). The morphologies and architectures of the UPE fibers at different drawing stages were characterized by polarizing optical microscope (POM), scanning electron microscope (SEM) and atomic force microscopy (AFM). The aggregation structure evolution of UHMWPE macromolecules during the high-ratio hot-drawing process was studied by differential scanning calorimeter (DSC), wide-angle X-ray diffraction (WAXD), small angle X-ray scattering (SAXS) and other testing methods. The experimental results demonstrated that the UHMWPE/decalin spinning suspension was extruded from the spinneret hole to form a fine spinning flow, followed by the formation of the transitional-state fibers at different processing stages, and finally the ready-made fibers. The total drafting ratio of the UPE fibers after fabrication reached more than 600 times. The diameter of the single UPE filament was reduced to 5.66 μm with elevated drawing ratios. The crystal structure of the prepared UPE fibers was progressively improved, and the folding-chain crystals of fibers gradually transformed into extended-chain crystals. The mechanical properties of the UPE fibers were significantly improved. The fracture strength of the as-spun UPE fibers reaches 48.1 cN/dtex, which endows the fibers with specific characteristics such as ultra-fine denier and ultra-high strength.

Nanoscale assembly of enantiomeric supramolecular gels driven by the nature of solvents.

Understanding the key parameters that control the self-assembly process is critical to predict self-assembly modes in multi-component systems, which will lead to the development of nanofibrous materials with tuneable properties. Enantiomeric amino acid-based low-molecular-weight gelators (LMWGs) were mixed in polar (polar protic) and aromatic apolar (aromatic) solvents and compared to their individual counterparts to probe the effect of solvent polarity on the self-assembly process. Scanning electron microscopy (SEM) reveals that xerogels of individual components display hollow needles in polar protic solvents, while chiral coils are observed in aromatic solvents. In contrast, the multi-component gel displays hollow needle morphologies in both solvents, indicating similar morphologies in polar protic solvents but an entirely different nanostructure for the individual gel networks in aromatic solvents. PXRD experiments performed on the dried gels showed that the nature of the solvents plays a vital role in the co-assembly process of multi-component gels. The self-assembly modes and the gel state structure of the gels are analysed by wide-angle X-ray diffraction (WAXS) and small-angle neutron diffraction (SANS), which reveals that the mixed gel undergoes different co-assembly modes depending on the nature of the solvent systems. This study shows that different co-assembly modes can be achieved for structurally similar components by varying the solvent polarity, demonstrating the importance of solvent choice in the self-assembly process of multi-component gels.

Lysine-based non-cytotoxic ultrashort self-assembling peptides with antimicrobial activity.

Peptide-based molecules and their hydrogels are useful materials for biomedical applications due to the reversible nature of their self-assembly as well as the diversity of nanostructures that can be created starting from low-molecular weight compounds. In this study, we have focused on comprehending the characteristics of fibrillar networks of l-lysine-based self-assembled dipeptide hydrogels with a focus on their antibacterial properties. For that purpose, l-lysine has been complemented with hydrophobic aromatic moieties coming from l-phenylalanine and benzyloxyxarbonyl N-capping. In addition, the peptide C-terminus is blocked with alkylamides of different chain lengths which introduces additional dispersive interactions and hydrophobicity. These materials were well characterized by transmission electron microscopy, scanning electron microscopy, wide-angle powder X-ray diffraction and oscillatory rheology. Finally, biocompatibility and antimicrobial tests were performed showing that these hydrogels are compatible with HEK 293 cells and present a remarkable antibacterial activity against both Gram positive (S. aureus) and Gram negative (E. coli) bacteria.

Atomistically informed hierarchical modeling for revisiting the constituent structures from heredity and nano-micro mechanics of sheath-core carbon fiber.

To better understand the heterogeneous anisotropic nanocomposite features and provide reliable underlying constitutive parameters of carbon fiber for continuum-level simulations, hierarchical modeling approaches combining quantum chemistry, molecular dynamics, numerical and analytical micromechanics are employed for studying the structure-performance relationships of the precursor-inherited sheath-core carbon fiber layers. A robust debonding force field is derived from energy matching protocols, including bond dissociation enthalpy calculations and rigid-constraint potential energy surface scan. Logistic long range bond stretching curves with exponential parameters and shifted force vdW curves are designed to diminish energy perturbations. The pseudo-crystalline microstructure is proposed and validated using virtual wide angle X-ray diffraction patterns and bond-orientational order parameters. The distribution or alignment features of the nanocomposite microstructures are collected from quantum chemical topology analysis and normal vector extractions. Non-equilibrium tensile loading simulation predicts the decomposed strain energy contributions, principal-axis modulus, strength limit, localized stress, and fracture morphologies of the model. Finally, an atomistically-informed stiffness prediction model combining numerical homogenization and analytical self-consistent Eshelby-Mori-Tanaka-type effective mean field micromechanics theory is proposed, giving a successful estimation of the overall stiffness matrix of the sheath-core carbon fiber system. The hierarchical models in combination with the carbonization reaction template will help in providing efficient and feasible schemes for the synergistic process-performance control of distinct types of carbon fiber.

Concentration-tuned diverse response to selective biogenic amines using a reusable fluorophore: monitoring protein-rich food spoilage.

Maintaining the freshness of food is essential for a healthy and quality life. Nevertheless, it remains a global challenge. Hence, an easy detection and monitoring protocol would be highly desirable. A cyanoacrylic acid (CAA)-based fluorophore is manifested as a reusable platform that responds diversely against different concentrations of selective aliphatic biogenic amines (BAs) in both solution and vapor phases. Slow spoilage of the protein-rich food is progressively monitored through emission shifts visible to the naked eye. This fluorophore provides easy and naked-eye detection of the BA vapor through a change in emission, i.e., red → orange → orange-yellow → cyan → green and quantum yield enhancement, which occur in stepwise increments of vapor concentrations. The probe design includes π-conjugated functionalized fluorescent molecules linked to multiple twisting sites, resulting in both solid and solution-state emission. The attached carboxylic acid responds quickly with selective BAs, mainly putrescine (PUT), cadaverine (CAD), and spermidine (SPM), where the concentration-based emission variation has appeared to be distinct and prominent against PUT [sensitivity (μM): 2 (solution); 3.3 (vapour)]. The selectivity towards diamine can be clarified by the formation of carboxylic acid salts and the consequent proton exchanges between free and protonated amines. In addition, -CN···H interaction is likely to develop within this ammonium carboxylate system, providing extra stability. Such ammonium carboxylate salt formation and gradual change in the molecular arrangement, resulting in symmetry development, are validated by FT-IR and wide-angle X-ray diffraction studies. Besides, this fact is supported by DFT studies that validate intramolecular H-atom exchange between free amine and ammonium salt units. A fluorophore-coated coverslip, filter paper, or silica gel-coated Al-plate is fruitfully utilized to detect the freshness of fish and chicken, which reveals the potential of this probe to prevent food waste and control food safety.

A facile strategy for the preparation of polylactide nano-microspheres with enhanced stereo-complexations.

Stereo-complexed polylactide (sc-PLA) nano-microspheres were separated by adding poor solvent to the poly(l-lactide) (PLLA)/poly(d-lactide) (PDLA) blend solution. The effects of different process parameters (concentration, processing method, ratio of PLLA/PDLA blend solution to poor solvent) on the microsphere particle size were investigated. The microscopic morphology, crystallinity, and thermal properties were investigated by Fourier transform infrared spectroscopy, differential scanning calorimetry, two-dimensional wide-angle X-ray diffraction, transmission electron microscopy and scanning electron microscopy. The results indicated that when the concentration reached 10 wt% and the PLLA/PDLA blend solution to poor solvent ratio was 1 : 5, the sc-PLA nano-microspheres exhibited more regular shape, good sphericity and uniform particle size, and the highest crystallinity. Additionally, the degree of crystallinity of the stereo-complexed crystals was as high as 39.60%, the rate of stereo-complexation was 99.65%, and the melting temperature reached 220 °C, indicating notable improvement in the crystallization and thermal properties. The sc-PLA nano-microspheres obtained in this research could be used as a nucleating agent for fibers and drug delivery carrier, and the sc-PLA nano-microspheres have broad application prospects in the textile and biomedical fields.

Elucidation of the Interplay between the Features of the Precursor and the Physicochemical Properties of “Core-Shell” Hierarchical Carbon Nitride Electrocatalysts for the Oxygen Reduction Reaction

The oxygen reduction reaction (ORR) is a major bottleneck in the operation of proton-exchange membrane fuel cells (PEMFCs) since it introduces large overpotentials (no less than 250-300 mV), which degrade significantly the energy conversion efficiency of the device. In addition, the electrocatalysts (ECs) yielding the lowest ORR overpotentials in the acidic environment found at the PEMFC cathode are based on Pt, a very scarce critical raw material (CRM). Pt raises concerns as it might trigger serious supply bottlenecks in the event of a practical widespread implementation of PEMFCs in the framework of today’s energy transition. Hence, the development of high-performing and durable ECs for the ORR is a major stepping stone towards the large-scale rollout of PEMFCs.In our research group a new breakthrough approach has been devised for the synthesis of ORR ECs, that is completely different form the preparation routes that are commonly adopted in the state of the art [1, 2]. Briefly, the approach consists in the pyrolysis and subsequent treatment of a precursor obtained by coupling suitable carbon species/sacrificial supports with a zeolitic inorganic-organic polymer electrolyte (Z-IOPE). The latter comprises anionic complexes including the Pt “catalyst” and other “co-catalysts”, which are bridged by organic binders [1,2].On one hand, the proposed approach has already shown its potential to yield ECs exhibiting a performance and durability improved with respect to Pt/C benchmark ECs. On the other hand, the proposed approach is extremely flexible, especially with respect to the synthesis of the initial EC precursor. In principle, it is possible to modulate a number of crucial features of such EC precursor, with a particular reference to: (i) the chemical composition (e.g., in terms of Pt, other “co-catalysts” and N; the latter plays a crucial role to stabilize the active sites into “coordination nests” on the EC surface, raising durability); and (ii) the morphology, that can be “templated” on suitable species (e.g., carbon species, sacrificial supports). The very flexibility of the proposed synthetic process needs to be leveraged appropriately to maximize the performance of the final ORR ECs, at the same time minimizing the efforts wasted on approaches with a low development potential.Herein it is elucidated how the modulation in the parameters involved in the synthesis of the EC precursor (e.g., the binder and the approaches to couple the Z-IOPE with the support) impact the physicochemical and electrochemical properties of the final ECs, with a particular reference to the chemical composition, morphology and distribution of the ORR active sites. An extensive characterization of the final ECs is carried out. Inductively-coupled plasma atomic emission spectroscopy (ICP-AES) and microanalysis are adopted to determine the bulk chemical composition. Near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) is used to elucidate the surface chemical composition and the chemical states of the surface elements. Ultra-high resolution scanning electron microscopy (UHR-SEM) and transmission electron microscopy (TEM) allow for the elucidation of EC morphology. The porosimetric features are probed by automatic gas adsorption instrumentations. Wide-angle X-ray diffraction (WAXD) is crucial to resolve the crystal structure. Cyclic voltammetry with the rotating ring-disk electrode method (CV-TF-RRDE) is used to clarify the “ex-situ” electrochemical performance and ORR reaction mechanism. Finally, the most promising ECs are used in the fabrication of single PEMFCs, that are tested as a function of the operating conditions.It is revealed that, in comparison with the Pt/C benchamark, some ECs are characterized by a much higher intrinsic kinetic performance due to the electronic and bifunctional effects bestowed by the carbon nitride support and the «co-catalysts». Finally, the binder has a marked effect on the stoichiometry, size, and distribution of the PtMx aggregates bearing the active sites.

Citryl-Imino-Chitosan Xerogels as Promising Materials for Mercury Recovery from Waste Waters.

The present study reported the obtention of xerogels based on chitosan and citral and their use as materials for mercury ion recovery from aqueous solutions, this being a serious problem related to the environment. The systems were prepared by the acid condensation of chitosan with citral, followed by the lyophilization of the resulting hydrogels, in order to obtain highly porous solid materials. The structural, morphological and supramolecular characterization of the systems was performed using 1H-NMR and FTIR spectroscopy, scanning electron microscopy and wide-angle X-ray diffraction. The ability of the obtained materials to be used for the recovery of mercury from aqueous solutions revealed the high potential of the xerogels to be used in this sense, the analysis of the materials post mercury absorption experiments revealing that this ability is predominantly conferred by the imine linkages which act as coordinating moieties for mercury ions.

Effects of moisture content and retrogradation on structure and properties of indica rice flour and starch gels

The physicochemical, functional, and sensory attributes of indica rice gels is strongly influenced by starch retrogradation. The objective of this study was to improve the cooking and textural qualities of indica rice gels by controlling retrogradation conditions. Differential scanning calorimetry (DSC), infrared spectroscopy (FITR), small angle X-ray scattering (SAXS), wide angle X-ray diffraction (XRD), and scanning electron microscopy (SEM) analyses showed that retrogradation modified the molecular interactions, increased the crystallinity, and altered the microstructure of indica rice gels. Retrogradation of rice gels in the presence of 40% moisture for 12 h significantly improved their cooking and rehydration properties. The rehydration rate of indica rice starch and flour gels increased by around 10.62% and 8.41%, while the cooking loss decreased by about 24.63% and 29.30%, respectively, compared to the non-retrograded controls. The textural attributes of these gels were also influenced by retrogradation: the tensile increased by 23.48% and 37.13%, the hardness increased by 37.30% and 29.86%, the springiness increased by 4.94% and 2.43%, and the adhesiveness decreased by 41.62% and 37.28%, respectively. The presence of protein in the indica rice flour significantly inhibited the degree of retrogradation. The results showed that control retrogradation can be used to enhance the cooking and quality attributes of indica rice gels. This knowledge may be useful for improving the properties of rice-based food gels.

Fabrication of high performance polyimide fibers by dry-jet wet spinning technology

High-performance co-polyimide (co-PI) fibers derived from 3,3`4,4`-biphenyldianhydride (BPDA), p-phenylenediamine (p-PDA) and 2-(4-aminophenyl)-5-amino-benzimidazole (BIA) were prepared via the wet spinning and dry-jet wet spinning method, respectively. The distinctions between wet spinning and dry-jet wet spinning processes on the structures and properties of co-PI fibers were systematically investigated. The co-PI fibers prepared by dry-jet wet spinning exhibited smoother surface morphology and higher mechanical properties than those of co-PI prepared by wet spinning. Wide-angle X-ray diffraction (WAXD) results showed that the co-PI fibers prepared by dry-jet wet spinning exhibited highly oriented structure along the fiber direction along with a low degree of lateral packing order in the transverse direction. Small-angle X-ray scattering (SAXS) revealed that the radius, length, misorientation and internal surface roughness of the microvoids in the co-PI fibers prepared by the dry-jet wet spinning are lower than those in co-PI fibers prepared by wet spinning. Moreover, the effect of air layer height, as well as the heat treatment on the structure and properties of fibers during the dry-jet wet spinning process, was also studied. The tensile strength and modulus of co-PI fibers prepared by dry-jet wet spinning reached 2.72 GPa and 114.29 GPa, respectively, with an air layer height of 10 mm and a heat stretching temperature of 440°C.

Photocatalytic Degradation of Ceftriaxone Using TiO2 Coupled with ZnO Micronized by Supercritical Antisolvent Route.

Heterogeneous photocatalysis is a promising technique for removing pollutants from water. In this work, supercritical antisolvent (SAS)-micronized ZnO (ZnOSAS) is coupled with commercial anatase TiO2 (PC50) to study the photocatalytic degradation of ceftriaxone under UV and visible light. Diffuse ultraviolet-visible reflectance (UV-vis DRS) measurement revealed that the presence of ZnO leads to a slight absorption in the visible region. Wide-angle X-ray diffraction (WAXD) analysis showed the presence of both ZnO wurtzite and TiO2 anatase crystalline phases in the composite. Photocatalytic tests proved that the activity of the ZnOSAS/PC50 composite is higher than that of commercial ZnO, SAS-micronized ZnO, and PC50, allowing complete ceftriaxone degradation under UV light after only 2 min of irradiation time. In contrast, about 90% of ceftriaxone degradation is achieved after 180 min of visible-light irradiation. The photocatalytic results for an experiment carried out in the presence of probe scavenger molecules for reactive oxygen species show that hydroxyl radicals and positive holes are both reactive species involved in the ceftriaxone photocatalytic degradation mechanism. Finally, reuse cycles of the ZnOsas/PC50 composite are performed, demonstrating the stability and recyclability of the photocatalyst.

Investigation of the Microstructure of PAN Precursor Fibers Obtained at Various Processing Stages

The production of high-performance carbon fibers relies heavily on the structural transformations of polyacrylonitrile (PAN) fiber during processing. In this article differential scanning calorimetry (DSC), synchrotron small-angle X-ray scattering (SAXS), and synchrotron wide-angle X-ray diffraction (WAXD) were used to study the changes of the thermal properties, voids and crystal structure of the PAN precursor fibers on industrial lines during the continuous processing stages, i.e., after the treatment in the coagulation bath, after stretching in boiling water and after stretching in high-temperature steam. The findings of this study suggest that after boiling water stretching the molecular chain motion of the PAN precursor fiber weaken, resulting in the expansion of the voids. After high-temperature steam stretching the voids became elliptical and oriented in the stretching direction. Although the boiling water stretching process partially damaged the (100) crystal planes of the PAN precursor fibers, it does not hinder their overall crystalline structure. The high stretching ratio primarily affected the orientation of the molecular chains. This orientation, even in the context of partial crystal plane disruption, further promoted the crystallization of the (100) crystal planes in the fibers. These experiments explored the correlation between the processing technology and fiber structure transformation of PAN-based carbon fibers, resulting in producing a guide for the preparation of high-performance carbon fibers with fewer defects.

Multi-scale investigation of the heat-induced transformation of starch in model dough and starch systems

Our study investigated the impacts of starch botanical origin (tapioca versus wheat starch) and gluten addition on the water distribution and hydrothermal changes of starch in model dough systems compared to their pure starch counterparts. In it, we employed a combination of time-domain nuclear magnetic resonance (TD-NMR), wide angle X-ray diffraction (WAXD), solid state nuclear magnetic resonance (ssNMR) at variable temperature (VT) and differential scanning calorimetry (DSC) measurements. The results showed that at intermediate hydration levels, water ingress into starch granules, increase in glucan chain mobility, and dissociation of double helices (DH) of amylopectin occurred at lower temperatures than crystallite loss of order and melting. The inhibitory effect of gluten on wheat starch hydrothermal changes was explained by a higher water adsorption capacity of gluten compared to starch at this hydration level (50%, wb). However this effect was shown to be influenced by starch botanical origin, tapioca-based systems showing no hindrance effect of gluten on starch-water interaction. The study also provides additional evidence for the sensitivity and detection scales of the different techniques at 50% water content.

Fabrication of Flexible Films for Supercapacitors Using Halloysite Nano-Clay Incorporated Poly(lactic acid).

In the past few years, significant research efforts have been directed toward improving the electrochemical capabilities of supercapacitors by advancing electrode materials. The present work signifies the development of poly(lactic acid)/alloysite nano-clay as an electrode material for supercapacitors. Physico-chemical characterizations were analyzed by Fourier transform infrared spectroscopy, wide-angle X-ray diffraction, and a universal testing machine. Cyclic voltammetry, electrochemical impedance spectroscopy, and galvanostatic charge-discharge techniques were employed to evaluate electrochemical characteristics. The optimized poly(lactic acid)/halloysite nano-clay film revealed the highest specific capacitance of 205.5 F g-1 at 0.05 A g-1 current density and showed 14.6 Wh kg-1 energy density at 72 W kg-1 power density. Capacitance retention of 98.48% was achieved after 1000 cycles. The microsupercapacitor device presented a specific capacitance of 197.7 mF g-1 at a current density of 0.45 mA g-1 with 10.8 mWh kg-1 energy density at 549 mW kg-1 power density.