Characterization Techniques Research Articles

A controlled co-assembly approach to tune temperature responsiveness of biomimetic proteins.

The controlled co-assembly of biomacromolecules through tuneable interactions offers a simple and fascinating opportunity to assemble multiple molecules into a single entity with enhanced complexity and unique properties. Herein, our study presents a dynamic co-assembled system using the multistimuli responsive intrinsically disordered protein Rec1-resilin and the adhesive hydrophilic protein silk sericin (SS). We utilized advanced characterization techniques including circular dichroism (CD) spectroscopy, dynamic light scattering (DLS), small-angle X-ray scattering (SAXS), and small/ultra-small angle neutron scattering (SANS/USANS) to elucidate the detailed co-assembly behavior of the system and its evolution over time and temperature. To achieve sufficient neutron contrast, we successfully biosynthesised deuterium-labeled Rec1-resilin (D-Rec1). Our research demonstrates that this co-assembly allows the formation of a robust entity with dynamic conformational assembly and disassembly, exhibiting both the upper critical solution temperature (UCST) and lower critical solution temperature (LCST) with reversibility. The assembly and disassembly dynamics of the co-assembled entity at UCST are very fast, while the process is kinetically controlled at LCST. This study provides significant new insights into the interplay of a hydrophilic, multi-responsive IDP and a highly hydrophilic protein, shaping the thermoresponsive and stable properties of the co-assembled entity.

High-performance single-atom M/TiO2 catalysts in the reverse water-gas shift reaction: A comprehensive experimental and theoretical investigation

Single-atom catalysts (SACs) offer high efficiency and selectivity in chemical reactions but face challenges in converting CO2 to CO via the reverse water gas shift (RWGS) reactions. This study addresses these challenges by anchoring three noble metals (Ir, Pd, and Ru) onto titania (TiO2) and analyzing their performance. Comprehensive characterization techniques, including electron microscopy, confirmed the uniform dispersion of metal atoms on TiO2. Among the catalysts, Ir/TiO2 exhibited the best results, achieving an 84 % CO2 conversion rate and ∼98 % CO selectivity, surpassing Pd/TiO2 and Ru/TiO2, which gained 56 % and 52 % conversion, respectively. In-situ gas transmission electron microscopy revealed the catalytic behavior of Ir/TiO2, showing Ir atom mobility and the formation of ∼1 nm nanoclusters. Density functional theory (DFT) and in-situ diffuse reflectance infrared spectroscopy (DRIFTs) further explained that the atomically dispersed Ir sites in Ir/TiO2 follow a hydrogen-assisted mechanism, with the COOH* intermediate desorbing and dissociating into CO. These findings suggest SACs' potential to facilitate greener chemical processes and reduce greenhouse gas emissions.

Feasible Preparation of Naphthalimide-Functionalized Zeolitic Imidazolate Framework-8 for Control, and Fluorescence Detection of Virus: Optimization of Model Study.

The onset of the coronavirus has highlighted the critical need to swift diagnostic techniques to identify the virus. Metal Organic Frameworks (MOFs) have attracted considerable attention in the field of sensing due to the remarkable characteristics. The present research examines the microwave preparation of naphthalimide-functionalized zeolitic imidazolate framework-8 (NI/ZIF-8) to the detection of coronavirus as a probe. The microwave synthesis approach facilitates an environmentally sustainable, and effective production of NI/ZIF-8. Characterization techniques have validated the material's high crystallinity and thermal behaviour. In order to enhance the performance of the probe, a 23 factorial model is implemented. This model facilitates the influences of control parameters, including NI/ZIF-8 dose, solution temperature, and buffer pH, on quenching response. The findings indicate the 27°C, pH 8.2, and a NI/ZIF-8 dose of 0.6mg/mL yields the maximum quenching response (83.21%). Additionally, it has been determined that photo electron transfer plays a significant role within the quenching process. The sensor demonstrated remarkable sensitivity to the COVID-19 RNA, achieving an exceptionally detection limit of 5.45 pM and a quick sense (20min), alongside a high detection selectivity of RNA. This project underscores the applicability of NI/ZIF-8 as an effective and eco-friendly sustainable substance for the rapid and accurate detection of RNA of COVID-19.

Observing Mixed Chemical Reactions at the Positive Electrode in the High-Performance Self-Powered Electrochemical Humidity Sensor.

Electrochemical humidity (ECH) sensors that integrate power generation and humidity sensing have attracted great research attention in recent years. However, the design of high-performance ECH sensors faces many challenges. Namely, the working mechanism of the ECH sensors is still controversial, and related self-powered applications have not been well implemented. To overcome these limitations, this study constructs an ECH sensor with high power-generation and humidity-sensing performance using the KCl/carbon black/halloysite nanotubes (KCl/CB/HNTs) as a humidity-sensing electrolyte. The proposed ECH sensor has a wide humidity-sensing response of 10.9%-91.5% relative humidity (RH), and a single ECH sensor can output 1.46 V with a maximum power of 133.2 μW at 91.5% RH. Particularly, the unprecedented mixed chemical reactions at the positive electrode, including the hydrogen evolution reaction and oxygen reduction reaction, are analyzed using multiple characterization and testing techniques. The analysis results provide solid experimental evidence for the current controversial working mechanism of ECH sensors. Due to the advantage of high-power generation, the proposed ECH sensor can be used for self-powered humidity detection. This study provides a valuable reference for improving the power generation of ECH sensors and solid evidence for clarifying their working mechanism, which could be beneficial for guiding the future development of ECH sensors.

Sustainable synthesis and environmental application of chitosan-Ocimum basilicum leaves-ZnO composite membrane for permanganate ion removal in wastewater treatment.

This study introduces a novel and environmentally friendly method for developing a cross-linked chitosan-Ocimum basilicum leaves-ZnO (ChOBLZnO) composite membrane, specifically designed for the adsorption of permanganate ions (MnO4-) from wastewater. Various characterization techniques, including Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Brunauer-Emmett-Teller (BET) surface area analysis, were employed to confirm the membrane's synthesis quality, structural integrity, and surface properties crucial for adsorption. The BET analysis revealed a surface area of 228.64 m2/g, indicating a highly porous structure. The membrane exhibited a high adsorption capacity of 142.8mg/g and an outstanding removal efficiency of 98.5%. The adsorption kinetics were best described by the pseudo-second-order model, with a correlation coefficient (R2) of 0.998, while the Freundlich isotherm model provided the most accurate fit for the adsorption behavior, with an R2 of 0.995. Thermodynamic studies indicated that the adsorption process is spontaneous and endothermic, with negative Gibbs free energy and positive enthalpy and entropy values. Reusability tests showed that the ChOBLZnO composite membrane maintained a high removal efficiency across five cycles, with minimal performance loss. These results demonstrate the ChOBLZnO composite membrane's potential as an efficient and sustainable solution for wastewater treatment, offering both high efficiency and durability.

Impact of Synthesis Parameters on the Crystallinity of Macroscopic Zeolite Y Spheres Shaped Using Resin Hard Templates

In this study, the effects of several synthesis parameters including aging time, micropore-structure-directing agents, and hydrothermal treatment temperature profile were systematically examined with respect to their impact on the crystallinity of macroscopic zeolite Y spheres formed in the presence of organic anion-exchange resin templates. Spherical resins were utilized as hard templates to shape the zeolite Y particles. Zeolite Y precursors were initially deposited into the pores of the resin template and subsequently crystallized over time through precise control over these synthesis parameters. The resulting zeolite Y spheres were characterized using an array of characterization techniques, including XRD, SEM, TEM, BET, FTIR, and XRF. We identify the optimal conditions for maximizing the crystallinity of the macroscopic zeolite Y particles using resin templates as macroscopic shaping agents. This functional material has the potential to be used as both catalyst and adsorbent in several applications.

Influence of radio-frequency magnetron sputtering power on electrical characteristics and positive bias stress stability of indium tin zinc oxide thin-film transistors

Abstract As the pursuit of high-quality display panels intensifies, the importance of high-performance thin-film transistors (TFTs) becomes increasingly prominent. Indium tin zinc oxide (ITZO) TFTs, as one of the promising directions for high-performance metal oxide TFTs, impose high demands on their performance and reliability. In this study, the performance and stability of ITZO TFTs fabricated under different radio-frequency magnetron sputtering power conditions were systematically tested and investigated. After sputtering power optimization, the field effect mobility of ITZO TFTs reaches 29.68 cm²/V·s, with a steep sub-threshold swing of 0.17 V/decade, near-zero threshold voltage, and good stability. Using atomic force microscopy and X-ray photoelectron spectroscopy characterization techniques, the thin films were analyzed to elucidate the relationship between sputtering power variations and oxygen vacancies.

Impact of niobium doping on photocatalytic degradation efficiency of iron oxide nanoparticles for methylene blue dye under UV and sunlight

Iron oxide (Fe2O3) nanoparticles were synthesized using lemon peel extract with niobium (Nb) doping (2, 4, and 6 mmol) via a hydrothermal method. Characterization techniques included FTIR, UV–Vis spectroscopy, XRD, PSA, and zeta potential measurement. FTIR confirmed Nb integration, with Fe-O and Nb-O bonds at 1.65 Å and 1.34 Å. Nb doping reduced particle size (93.74 nm to 56.01 nm) and enhanced stability (zeta potential −13.04 to −37.31 mV). XRD analysis confirmed phase purity and crystalline structure, while the Scherrer and Williamson-Hall methods revealed decreases in crystallite size and lattice strain with higher Nb concentration. Bandgap analysis showed a red shift (3.08 to 2.28 eV) due to Nb-doped energy levels. Nb-doped Fe2O3 (6 mmol) achieved 87 % degradation of methylene blue (10 ppm) under sunlight in 2 h. Enhanced photocatalysis resulted from prolonged electron-hole recombination, generating reactive radicals. These Nb-doped Fe2O3 nanostructures are promising for pollutant degradation in water environments.

Adsorption of perfluorosulfonic acids (PFSAs) on an ultrafine potato peel waste grafted β-cyclodextrin (UFPPW-β-CD)

Per- and polyfluoroalkyl substances are widely used in various consumer products. However, these compounds can cause various harm to the environment and health. Considering the high chemical stability, these compounds are not completely removed from the aqueous environment, and consequently, recent studies have detected their presence in water bodies. In this scenario, biomass-based adsorbents are promising. β-cyclodextrin (β-CD) was grafted in an ultrafine potato peel waste (UFPPW) to produce a novel, efficient and sustainable adsorbent (UFPPW-β-CD) that was used to remove three different perfluorosulfonic acids (PFSAs) from water. The efficient grafting was proved by several characterization techniques, which also demonstrated the main UFPPW-β-CD features. The UFPPW-β-CD was efficient for all PFSAs (perfluorohexanesulfonic acid (PFHxS), perfluoropentanesulfonic acid (PFPeS), and perfluorobutanesulfonic acid (PFBS)), with removal percentage higher than 74 %. The increase in the CF chain of PFSAs favored the adsorption due to the host–guest hydrophobic interactions between the CF chains of the adsorbates and the hydrophobic cavity of the β-CD. Removal percentages and adsorption capacities at pH 3.0 were 74.6 % (49.92 µg g−1) to the PFBS, 82.6 % (65.66 µg g−1) to the PFPeS, and 90 % (100.89 µg g−1) to the PFHxS. The kinetic followed the General order model, while the equilibrium agreed with the Sips isotherm. The adsorption capacity increased with the increase in the CF chain of the adsorbate, but the adsorption rate followed the opposite trend. PFSAs adsorption on the UFPPW-β-CD adsorbent was favorable and exothermic. UFPPW-β-CD could be used seven times, keeping its maximum adsorption capacity constant using ultrasound-assisted desorption. It can be concluded that UFPPW-β-CD is a sustainable adsorbent to uptake PFSAs from water, and this process is dependent on the size of the CF chains.

Titanium Nitride-Gold Nanoislands: Harnessing Electrical and Optical Properties for Enhanced Localized Surface Plasmon Resonance Sensing

Titanium nitride-gold nanoislands (TANIs) are experimentally investigated to explore their electrical and optical properties induced by the incorporation of Au into TiN. A film is first fabricated on a glass substrate using the radio frequency (RF) magnetron sputtering technique at 300 K, with a thickness of approximately 20 nm (± 2.5 nm) and an Au:TiN ratio of 0 to 0.47. Subsequent thermal annealing provides a nanoisland structure of TiN-Au. Characterization techniques such as X-ray diffraction and X-ray photoelectron spectroscopy confirmed the presence of TiN and Au in the fabricated TiN-Au nanoislands. Spectroscopic ellipsometry measurements show that the TANIs posses excellent optical properties. Furthermore, numerical evaluations of energy dissipation are conducted to assess carrier transport deterioration due to the inelastic scattering effects in the TANIs and the inclusion of Au in the nanostructure significantly have reduced the dielectric loss tangent at energies greater than 4.5 eV, compensating for high losses and enhancing optical performance. The biosensing capability of TANIs is also demonstrated with the sensing of biotin, such that a strong biotin-phase response relationship is formed with a limit of detection of 0.842 ng/ml. This study contributes valuable insights into the electrical, optical and biosensing properties of TANIs, providing direction for sensing applications, where the optimization of the TANIs structure could bring about advancements in optical performance and pave the way for the potential design of novel plasmonic sensors.

Adsorption mechanism of soy protein amyloid fibrils with different morphological structures at the interface of oil-in-water emulsion

Under specific processing conditions, globular food protein can form amyloid fibrils with excellent functional properties in food processing. Amyloid fibrils can be adsorbed on the surface of oil droplets to improve the stability of oil-in-water emulsion. The protein can form monomers oligomers, protofibrils and mature fibrils of which the concentrations increase with the prolonging acidic-heating time. However, the structural advantages of these aggregates when adsorbing at oil-water interface are unclear and the emulsifying ability and adsorption mechanism of food protein amyloid fibrils with different morphology at oil-water interface need to be studied in depth. Herein, four kinds of soy protein amyloid fibrils (SAFs) with distinct morphology were prepared by changing the acidic heating time (3, 6, 12 and 24 h), which were referred as SAFs-3, SAFs-6, SAFs-12 and SAFs-24. Their interfacial adsorption behavior at the oil-water interface were studied systematically by three-phase contact angle, interfacial tension, CLSM, Cryo-SEM and other characterization techniques. The results suggested that the length and flexibility of the fibrils have a great influence on the interface properties, including the rheological properties such as viscosity and modulus. These properties determine the emulsifying capacity of the fibrils. The emulsion stabilized by SAFs-12 was the most resistant to coalescence because SAFs-12 formed a stronger interfacial layer around the oil droplets and a denser viscoelastic network in the continuous phase. In our study, a stabilizing emulsion was prepared using SAFs, which provided potential applications for amyloid fibrils in the food field.

Synergistic regulation of dual thresholds: Hydroxyl occupancy and carbon species in the targeted catalytic hydrocracking of lignite

The preparation of carbon-based catalyst supports from low-grade lignite, followed by its self-catalytic hydrocracking to produce lignite-derived aromatic compounds, is crucial for achieving efficient lignite utilization and expanding aromatic compound sources. During lignite catalytic hydrocracking, the uncontrolled diffusive migration of active hydrogen (H*) and insufficient protection of aromatic rings reduce the yield of aromatic compounds. Using Heishan lignite as the raw material, we employed a relay process of thermal-induced self-assembly and oxidation-mediated carbon distortion for fabricating the Co3O4/AC&GC-S-600 composite material, which features an optimal hydroxyl occupancy ratio and a balanced combination of amorphous carbon/graphite carbon (AC/GC) types. The optimal hydroxyl occupancy threshold balances Co3O4 dispersion and hydrophilicity, facilitating the efficient formation and directional migration of H* through synergistic interaction between Co3O4 and H2O. The adequate threshold of AC/GC ratio regulates substrate adsorption, activation, and inhibition of aromatic hydrogenation, enhancing selective C–O bridge bond cleavage and preserving the unsaturation of aromatic rings. The synergistic regulation of dual thresholds promotes the rapid formation and the directional migration of H*, enabling efficient conversion of Heishan lignite to aromatic compounds (45.8% conversion, 80.8% selectivity) under mild conditions. Characterization techniques, experimental analyses, kinetic studies, and density functional theory calculations confirm that thermally induced self-assembly and oxidation-mediated carbon distortion are crucial for redistributing the carbon framework of the Heishan lignite matrix and regulating the optimal dual thresholds of hydroxyl occupancy and AC/GC types, which are essential for the catalytic hydrocracking of Heishan lignite to aromatic compounds. This strategy provides a scientific basis for selective catalytic production of lignite-based aromatic compounds, thereby supporting its clean and efficient utilization.

Co–Ni nanoparticle supported on heteroatom-doped carbon derived from garlic powder and eutectic solvent: Its application in Nitroarenes reduction

This paper presents the synthesis of a novel heterogeneous catalyst, PSN-C600-Co2:Ni1, designed for the hydrogenation of nitroaromatic compounds. The catalyst is a porous carbon substrate triply doped with nitrogen, sulfur, and phosphorus, incorporating bimetallic Co and Ni nanoparticles. A natural precursor, garlic biochar, and a biodegradable eutectic solvent were used in the synthesis. Various characterization techniques, including Scanning Electron Microscope (SEM), X-Ray Energy Diffraction Spectroscopy (EDX), Elemental Mapping Measurements (MAP), Thermogravimetric Analysis (TGA), X-Ray Diffraction (XRD), Infrared Spectrometer (FTIR), Transmission Electron Microscope (TEM), Raman Spectroscopy, and Nitrogen Adsorption and Desorption Pattern (N2 adsorption-desorption isotherm), were utilized to examine the features and properties of the synthesized PSN-C600-Co2:Ni1 catalyst.

High-pressure CO2 adsorption on MCM-41: Efficiency of microwave-assisted synthesis

The rapid increase in atmospheric CO2 concentrations, driven by human activities, has become a critical factor in global climate change, posing severe risks to sustainable development. Addressing this challenge necessitates substantial CO2 removal, which demands innovative and efficient technologies. Carbon dioxide adsorption on porous materials is a promising strategy to mitigate this issue. This study investigates the synthesis of ordered mesoporous silica MCM-41 by microwave irradiation, a technique that offers significant advantages over conventional hydrothermal methods. By optimizing the synthesis conditions, we produced MCM-41 silica with superior structural properties in just 30 min. Characterization techniques, including X-ray diffraction, FTIR, N2 adsorption/desorption isotherms, and transmission electron microscopy, confirmed the formation of well-defined pores and hexagonal channels. Notably, the synthesized MCM-41 exhibited a high CO2 adsorption capacity of 12.78 mmol g−1 at 25 °C and 50 bar, outperforming silicas produced via conventional methods and comparable to amine-modified silicas. These results highlight the potential of microwave-assisted synthesis to improve CO2 capture efficiency, offering a promising approach for future carbon capture and storage applications.

Composite Shell Microcapsules With Room Temperature Phase‐Change Properties and High Thermal Storage Density

AbstractInorganic hydrated salts, noted for their high thermal storage density, excellent thermal conductivity, and non‐toxicity, are suitable candidate material for thermal management, particularly in enhancing human living environments when their phase transition points are near room temperature. Herein, we present an efficient and environmentally friendly microencapsulation method for inorganic hydrated salt through organic phase separation method. Eutectic hydrated salt (EHS) consisted of sodium carbonate decahydrate (SCD) and disodium hydrogen phosphate dodecahydrate (DHPD) was prepared as the core material while the mixture of ethyl cellulose (EC) and acrylonitrile‐butadiene‐styrene (ABS) as composite shell materials. Various characterization techniques were used to evaluate the micromorphology, chemical structure, thermal properties and thermal stability of the microcapsules. The resulting microcapsules exhibited a phase change temperature of 22.6 °C with a remarkable enthalpy of 131.4 J/g. Particularly, the enthalpy remained at 117.7 J/g even after 50 thermal cycles, indicating stable cycling thermal reliability. Furthermore, it was confirmed that the EHS was effectively encapsulated within the composite shell, and the microcapsules had a quasi‐spherical shape and core‐shell structure. More importantly, this method of microencapsulation could potentially be extended to other liquid hydrated salts at room temperature, offering a versatile approach for future applications.

Transforming waste into multifunctional nanomaterials: Mg-doped carbon dots from cow dung for Y(III) detection and biomedical applications

Rare earth metal Yttrium (Y3+) plays a vital role in many electronic devices however, discarding these devices eventually contaminates the environmental sources. Herein, we have developed a Mg-doped carbon dots (M-CDs) as a fluorescent probe for selective and sensitive determination of Y3+ in water bodies. The M-CDs having maximum emission at 420 nm upon 310 nm excitation with 20 % quantum yield and which was synthesized from upcycling of agricultural waste i.e., cow dung by simple carbonization followed by hydrothermal method. M-CDs were confirmed using different analytical and characterization techniques as well as stable in different pH and ionic strength solutions. The M-CDs was highly selective towards Y3+ ions over different metal ions with significant blue shift. This fluorescent probe performs a good linear relationship between the different concentrations of Y3+ ion and fluorescence intensity (R2 = 0.99) within the range of 0.2 to 20 μg/mL with a detection limit of 0.019 µg/mL. The study indicates quenching of Y3+ was result of dynamic quenching and the Inner Filter Effect (IFE) effect. Also, the cytotoxicity of M-CDs was checked via CAM assay and significant growth in blood vascularization with healthy growth of chick embryo confirmed the M-CDs were biocompatible. The nontoxic M-CDs was employed for MCF-7 breast cancer cell imaging which gives bright blue fluoresce under UV light excitation. Further, aiming to a circular economy approach the residual carbon remaining after hydrothermal was used as reactivated carbon for the abatement of environmental pollutants. The sustainable, cost-effective and agricultural waste-derived Mg-doped CDs have potential applications in analytical, environmental, forensic as well as biomedical fields.

Optimizing n-heptane isomerization: The role of copper in enhancing the catalytic activity and selectivity of Pt and Cu-Pt/montmorillonite K10 catalysts

The development of efficient catalysts for n-heptane isomerization is essential for enhancing gasoline octane numbers. In this study, Pt and Cu-Pt/Montmorillonite K10 (MMT) catalysts were prepared and evaluated to investigate the effect of copper on catalytic performance and selectivity in the isomerization of n-heptane. Comprehensive characterization techniques, including XRD, BET, FTIR, TEM, and TPR, were used to investigate the structural, chemical, and electronic properties of the catalysts. Catalytic performance was tested in a fixed-bed reactor over a temperature range of 200 °C to 450 °C, with a liquid hourly space velocity (LHSV) of 1 h−1 and an H2/n-heptane ratio of 20 mL−1. The Pt/MMT catalyst exhibited an isomerization yield of 23.5 % and a selectivity of 66.8 % at 350 °C. In contrast, the incorporation of Cu into the Pt catalyst (0.8Cu-0.1Pt/MMT) enhanced its electronic environment, resulting in a higher isomerization yield of 29.6 % and selectivity of 77.5 % at the same temperature. Additionally, the Cu-Pt/MMT catalyst demonstrated robust long-term stability, maintaining an isomer yield of approximately 28.1 % and selectivity of 75.3 % after 50 h of continuous operation at 350 °C. This study highlights the improved performance of the Cu-Pt/MMT catalyst and offers valuable insights for optimizing bimetallic catalysts in hydrocarbon isomerization applications.

Outstanding electrocatalytic activity and corrosion property of NiCr nanoparticle alloys electrodeposited from a choline chloride/urea deep eutectic solvent

Nickel-chromium alloys are known for their superior corrosion resistance, wear resistance, and hardness, making them a topic of significant interest. This study explores the electrodeposition of Ni-Cr alloys onto a glassy carbon electrode from a choline chloride/urea deep eutectic solvent. Electrochemical techniques, including cyclic voltammetry and chronoamperometry, were utilized to explore the deposition process. Voltametric analysis revealed that Ni-Cr alloys could be electrodeposited from the reline DES through a single potential step. The analysis of current density transients indicated that the electrocrystallization of Ni-Cr follows a three-dimensional (3D) nucleation and diffusion-controlled mechanism on the bimetallic growing surface. Additionally, the presence of the Ni(II) component was found to significantly enhance the kinetics of Ni-Cr phase formation, facilitating rapid deposition from the eutectic mixture. Surface characterization techniques, including scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) mapping, and X-ray diffraction (XRD), confirmed the uniform distribution of elements, the formation of the Ni-Cr phase, and its crystalline structure. The high quality of nickel-chromium alloys obtained from DES highlights their potential applications in various engineering fields, particularly in surface coating and metal protection.

A comparative study of LiTa2PO8 ceramics prepared with different lithium sources

In advancing lithium-ion batteries, solid electrolytes like LiTa2PO8, a Li-ion conductor with high bulk conductivity (~10−3 S/cm), show promise for all-solid-state battery technology. Here, we investigate the impact of different Li sources and their excess on the structural, microstructural and electrical properties of LiTa2PO8 ceramics. Employing diverse characterization techniques, including XRD, MAS NMR, TMA, SEM/EDS, IS, DC potentiostatic polarization, and density measurements, we unveil significant impact of the source of lithium ions and its excess on electrical properties. The sample without excess LiNO3 source exhibited the highest σtot = 5.2×10−4 S/cm at 30°C. Notably, the grain conductivity remained constant at ca. 3 mS/cm, irrespective of the chosen lithium source and excess. The microstructural analysis uncovered correlations between variations in total ionic conductivity and changes in the nature and concentration of secondary phases. Additionally, it revealed the influence of the arrangement of grains affecting the grain boundaries and porosity regions.

Leveraging solid solubility and miscibility of etoricoxib in Soluplus® towards manufacturing of 3D printed etoricoxib tablets by additive manufacturing

This research focuses on exploring the solid solubility and miscibility of Etoricoxib, a poorly water-soluble anti-inflammatory drug, within Soluplus®, a polymer used as a matrix for 3D-printed tablets. By utilizing hot-melt extrusion (HME), the drug was dispersed within Soluplus® to enhance its solubility. The extrudates were then employed in 3D printing to create customized solid oral dosage form. This study’s novelty lies in combining HME and 3D printing, aiming to improve drug incorporation, stability, and effectiveness in the final formulation. Comprehensive characterization techniques, including hot stage microscopy (HSM), scanning electron microscopy (SEM), micro-computed tomography (Micro-CT), florescence microscopy, optical microscopy, X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), solubility studies, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), and aqueous solubility study were utilized to elucidate the physicochemical properties, thermal stability, and structural integrity for the extruded filaments (the printing ink), and 3D printed tablets made thereof. Furthermore, the in vitro drug release profile of the 3D printed tablet was systematically evaluated, revealing a controlled drug release pattern from the finished dosage form. The systematic investigation reported herein, starting from theoretical miscibility to the printing ink development through HME, detailed characterization of the extruded filaments, and further solid oral formulation development by additive manufacturing can be utilized as a platform technology or a pathway for the development of personalized medicine with drugs having similar physicochemical properties.