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This manuscript shows an innovative water-based processing route to fabricate lead-free piezoceramics. It faces the challenge of substituting conventionally used organic solvents by innocuous water. The procedure involves two methods of widespread use in industry: attrition ball-milling and freezing-lyophilization. Powders with nominal composition (Ba 0.92 Ca 0.08)(Ti 0.95 Zr 0.05)O 3 were effectively obtained. A narrow monomodal size distribution (600 nm) proved high reactivity that allowed solid-state synthesis at ultra-low temperature (700 °C-2 h). Optimal two-step sintering method (900 °C-3 h,1280 °C-6 h) allowed well-sintered homogeneous ceramics with pure tetragonal perovskite phase. They showed high piezo-sensitivity (d 33 =320 pC/N, d 31 =−110 pC/N, k p =31.45% and N p =2750 kHz·mm, ε ′ 33 T =3670, tanδ=0.036 at 1 kHz), comparable to that found for routes in organic media. Therefore, attrition ball milling in water and lyophilization work in synergy to successfully activate the precursors, influencing on the structural, microstructural and electrical properties of the final BCZT ceramics. This is an unprecedented development to produce piezoelectric ceramics using a sustainable, environmentally benign water-based process, with a positive impact in noteworthy industrial applications. • Novel mixed oxides route to fabricate (Ba 0.92 Ca 0.08) (Ti 0.95 Zr 0.05) O 3. • Attrition ball-milling in water, freezing and lyophilization activate the precursors. • Fine lyophilized powder (600 nm) allows ultra-low synthesis at 700 °C. • Two-step sintering at 1280 °C results in a pure tetragonal perovskite phase. • High piezo-sensitivity, alike that obtained by milling in organic media. [ABSTRACT FROM AUTHOR]

Though ferulic acid presents great hypoglycemic potential, it possesses limited aqueous solubility, and low oral bioavailability. When associated with metformin, the first-choice drug in Type 2 diabetes treatment, FA demonstrates synergistic hypoglycemic effects, however, it also causes certain undesirable dose-related effects. This study aimed to develop a new ferulic acid - metformin multicomponent system, and incorporate it into a solid dosage form with improved biopharmaceutical parameters. A novel metformin: ferulate (1:1) salt (MFS) was produced, which was properly characterized using differing analytical techniques, including single crystal analysis. Also during the course of the study, a new polymorph of the metformin free base was observed. The MFS was obtained using solvent evaporation methods, which achieved high yields in reproducible process, as well as a 740-fold increase in ferulic acid aqueous solubility. The MFS tablets developed met quality control requirements for this dosage form, as well as revealing excellent performance in vitro dissolution tests, presenting dissolution efficiency values of 95.4 ± 0.5%. Additionally, physicochemical instability was not observed in a study at 40 °C for 3 months for both MFS powder and its tablet form. The MFS product developed is a promising candidate for further Type 2 diabetes clinical study. [Display omitted] • A salt formation increases the aqueous solubility of the ferulic acid. • A new metformin free base polymorph is found. • Study of powder flow properties and formulation development are highlighted. • In vitro dissolution tests can provide the performance of metformin tablets. [ABSTRACT FROM AUTHOR]

Herein was demonstrated the facile solid-state synthesis of ZnS/ZnO nanocomposites using planetary ball milling followed by subsequent thermal treatment. X-ray diffraction analysis has shown that the ZnS/ZnO products are nanocrystalline with an estimated crystallite size of less than 60 nm. A transmission electron microscope has demonstrated the presence of spherical heterostructures and core-shell structured ZnS/ZnO nanocomposites with the size being 40–80 nm in diameter. Fourier transform infrared spectroscopy analysis confirmed the presence of Zn–O and Zn–S bonds. The formation of a thin boundary between the ZnS and ZnO phases, where the sulfur oxidation state varies from −2 to +6, was determined by X-ray photoelectron spectroscopy. Degradation of methylene blue and Orange II organic dyes was used to assess the photocatalytic activity of ZnS/ZnO nanocomposites, and the nanocomposites of ZnS/ZnO, with a mass ratio of ∼1:1, demonstrated the highest visible light photocatalytic activity. For photocatalytic hydrogen production experiments, the surface of ZnS/ZnO nanocomposites was in situ decorated with NiS nanoparticles, where the mass content of NiS was 1.5%. The presence of NiS cocatalyst promotes the separation and transfer of photogenerated charges, thereby increasing the photocatalytic activity of ZnS/ZnO nanocomposites during hydrogen generation. The apparent quantum efficiency of photocatalytic hydrogen generation using ZnS/ZnO-3h-NiS photocatalyst was equal to 1.13%. This contribution shows the possibility to prepare nano-structured photocatalysts via mechanochemistry. [Display omitted] [ABSTRACT FROM AUTHOR]

• A 23-tube, single-stage staggered active elastocaloric regenerator was developed. • Fluid-solid ratio, (un)loading time, and strain significantly impact performance. • A maximum temperature span of 16.6 K was achieved at zero load conditions. • Nitinol tubes withstood over 30,000 cycles without failure. Elastocaloric solid-state refrigerants have a lower environmental impact compared to conventional vapor compression refrigerants, but they require significant advancements to gain widespread implementation. Two barriers that prevent adoption are the low-temperature lift and poor fatigue life. This paper presents a compression-loaded, staggered-tube active elastocaloric regenerator designed to address these challenges, along with the optimal operating parameters for the system. We conducted a sensitivity analysis on a single-stage device and identified fluid-solid ratio, cycle time, and applied strain as key factors affecting thermal response. Test results for the regenerator yielded a maximum steady-state temperature span of 16.6 K (9.7 K in heating and 6.8 K in cooling) at 4% strain and under zero load conditions, over two times larger than the baseline value. The tubes also withstood over 30,000 cycles without failure. The outcomes shown in this paper contribute to the foundation—in both design and operating conditions—of growing works aimed at demonstrating high-performing caloric devices. [ABSTRACT FROM AUTHOR]

Cocrystallization is a technique for improving the physical properties of active pharmaceutical ingredients. However, cocrystals can transform into more stable polymorphs as well as dissociate to original materials. Therefore, an analytical technique is required to determine the polymorphic transformation quickly and accurately in tablets. The purpose of this study is to develop a method to monitor cocrystal polymorphs in model tablets using transmission low-frequency Raman spectroscopy. The tablets, consisting of only metastable polymorphs of caffeine-glutaric acid cocrystals, were stored under various relative humidity levels. The composition of the cocrystal polymorphs were calculated from a calibration curve relating the actual composition to the predicted values calculated by partial least squares regression processing of low-frequency Raman spectra. The metastable form gradually converted to a stable form, and polymorphic phase transformation occurred with increasing relative humidity. Ninety-six percent of the metastable form converted into a stable form stored at 25 °C after 3 h at 95% RH. In conclusion, transmission low-frequency Raman spectroscopy can be used to quantitatively monitor cocrystal polymorphs. This technique is one of the candidate techniques to quantifiably evaluate the physico-chemical stability of cocrystal polymorphs in tablets. Graphical Abstract [Display omitted]. • This is the first report that successfully quantifies cocrystal polymorphs using low-frequency Raman spectroscopy. Quantification of cocrystal polymorphs has not been achieved by conventional analytical methods because it requires solid-state analysis. • We also demonstrate the use of the method for stability monitoring of active pharmaceutical ingredients in formulations. • Based on these results, we suggest the use of transmission low-frequency Raman spectroscopy for solid-state analysis of cocrystal polymorphs in pharmaceutical formulations. [ABSTRACT FROM AUTHOR]

[Display omitted] • The effective approach for high-quality solid-state VCD spectra was suggested. • The cluster and transfer approach to calculate solid-state VCD was adapted. • Structures of three polymorphs of sofosbuvir and its cocrystal were studied by solid-phase VCD. X-ray diffraction is a commonly used technique in the pharmaceutical industry for the determination of the atomic and molecular structure of crystals. However, it is costly, sometimes time-consuming, and it requires a considerable degree of expertise. Vibrational circular dichroism (VCD) spectroscopy resolves these limitations, while also exhibiting substantial sensitivity to subtle modifications in the conformation and molecular packaging in the solid state. This study showcases VCD's ability to differentiate between various crystal structures of the same molecule (polymorphs, cocrystals). We examined the most effective approach for producing high-quality spectra and unveiled the intricate link between structure and spectrum via quantum-chemical computations. We rigorously assessed, using alanine as a model compound, multiple experimental conditions on the resulting VCD spectra, with the aim of proposing an optimal and efficient procedure. The proposed approach, which yields reliable, reproducible, and artifact-free results with maximal signal-to-noise ratio, was then validated using a set comprising of three amino acids (serine, alanine, tyrosine), one hydroxy acid (tartaric acid), and a monosaccharide (ribose) to mimic active pharmaceutical components. Finally, the optimized approach was applied to distinguish three polymorphs of the antiviral drug sofosbuvir and its cocrystal with piperazine. Our results indicate that solid-state VCD is a prompt, cost-effective, and easy-to-use technique to identify crystal structures, demonstrating potential for application in pharmaceuticals. We also adapted the cluster and transfer approach to calculate the spectral properties of molecules in a periodic crystal environment. Our findings demonstrate that this approach reliably produces solid-state VCD spectra of model compounds. Although for large molecules with many atoms per unit cell, such as sofosbuvir, this approach has to be simplified and provides only a qualitative match, spectral calculations, and energy analysis helped us to decipher the observed differences in the experimental spectra of sofosbuvir. [ABSTRACT FROM AUTHOR]

Developing earth-abundant, low-cost, high-efficiency electrocatalysts for hydrogen evolution reaction (HER) by structure design is still a grand challenge. Herein, we fabricated Ni nanoparticles encapsulated by carbon loaded in two-dimensional carbon nanosheets (2D Ni@C@SU) using a molten salt (NaCl)-assisted pyrolysis method. Because of the large specific surface area (262.35 m²/g) and high electrical conductivity, the prepared 2D Ni@C@SU-0.75 electrocatalyst exhibits excellent HER electrocatalytic activity with the overpotential of −105 mV at −10 mA cm−2 and −367 mV at −200 mA cm−2, which is close to the commercial benchmark Pt/C (η 200 = −339 mV). Besides, the catalyst displays incredible durability in the electrocatalytic HER. This research indicates that the green solid-state synthetic strategy provides a new window for designing new Ni-based composite catalysts for electrocatalytic HER. [Display omitted] • Catalysts were prepared by a facile one-step synthesis. • The synthesis process is green and solvent-free. • Ni@C@SU-0.75 catalyzes hydrogen evolution reaction with -105 mV at 10 mA/cm2, and exhibited a good stability. • The 2D nanosheets encapsulated structure can increase the active sites and promote proton/electron transport. [ABSTRACT FROM AUTHOR]

We compared "ice-fog" controlled ice nucleation at -6 °C to annealing at the same temperature for a 50 mg/mL monoclonal antibody formulation, using shelf-ramp freezing as a control. Cake structure, drying time, reconstitution time, specific surface area, calculated cake resistance and size exclusion chromatography were all compared. Controlled nucleation resulted in the fastest reconstitution, shortest primary drying, lowest calculated cake resistance, lowest specific surface area and highest moisture content. There was no effect upon the results for size exclusion chromatography. Results for annealing were between those for controlled nucleation and shelf-ramp freezing. All results were consistent with "ice-fog" controlled nucleation at -6 °C having greater impact upon the ice crystal morphology than annealing at the same temperature for 3 h. [ABSTRACT FROM AUTHOR]

Lipid-based systems have many advantages in formulation of poorly water-soluble drugs but issues of a limited solvent capacity are often encountered in development. One of the possible solubilization approaches of especially basic drugs could be the addition of fatty acids to oils but currently, a systematic study is lacking. Therefore, the present work investigated apparently neutral and basic drugs in medium chain triglycerides (MCT) alone and with added either caproic acid (C6), caprylic acid (C8), capric acid (C10) or oleic acid (C18:1) at different levels (5 – 20%, w/w). A miniaturized solubility assay was used together with X-ray diffraction to analyze the residual solid and finally, solubility data were modeled using the conductor-like screening model for real solvents (COSMO-RS). Some drug bases had an MCT solubility of only a few mg/ml or less but addition of fatty acids provided in some formulations exceptional drug loading of up to about 20% (w/w). The solubility changes were in general more pronounced the shorter the chain length was and the longest oleic acid even displayed a negative effect in mixtures of celecoxib and fenofibrate. The COSMO-RS prediction accuracy was highly specific for the given compounds with root mean square errors (RMSE) ranging from an excellent 0.07 to a highest value of 1.12. The latter was obtained with the strongest model base pimozide for which a new solid form was found in some samples. In conclusion, targeting specific molecular interactions with the solute combined with mechanistic modeling provides new tools to advance lipid-based drug delivery. [ABSTRACT FROM AUTHOR]

In this investigation, (Gd x Y 1-x)VO 4 :Er3+ (x = 0, 0.25, 0.5, 0.75, 1) compounds were synthesized via a facile solid-state method at 1100 °C. The XRD results clarified that the increase of Gd element gives rise to the left shift of diffraction peaks. The employment of SEM revealed that the ratio of Gd/Y significantly influences the microstructure while the smallest particle size of phosphors (∼2 μm) was achieved in GdVO 4 luminescent material. The photoluminescence characterization confirmed that the highest excitation intensity is occurred at the wavelength of 310 nm while the corresponded emission spectrum consists of two strong peaks at the approximate wavelengths of 534 and 562.5 nm, which are attributed to 2H 11/2 -4I 15/2 and 4S 3/2 -4I 15/2 , respectively. Finally, it was interestingly concluded that the strongest emission intensity belongs to GdVO 4 phosphor material. The adsorption spectra proved that the employment of ball milling efficiently enhances the adsorption characteristics. [ABSTRACT FROM AUTHOR]

The transition towards more sustainable industrial processes implies proposing alternative technologies to help resolving the environmental issues attributed to the industrial sector. This paper presents some aspects of the microwave-assisted technology which, if correctly applied from the R&D phase and up to the industrial scale, may lead to significant savings in energy consumption, process time and environmental remediation connected with industrial processing and process intensification. This article is intended to the development of a more detailed knowledge of the specific elements of the microwave technology and of the practical issues associated with processing using microwaves as to enable a better understanding of microwave-assisted processes and what it takes to scale them up. • Sustainable industrial processes require new technologies and production methods. • Microwaves are an alternative to replace conventional energy in industrial processing. • Applications of microwaves in the chemical industry are scarce. • Solid-state microwave generators can be a disruptive force in multiple markets. • Microwave energy transfer to a product can be controlled precisely. [ABSTRACT FROM AUTHOR]

• Eu3+ doped CaMoO 4 nanopowders were synthesized using Solid-state synthesis technique. • DRS spectra indicate the band gap energy values range between 4.63 – 5.32 eV. • Hexagonal rod-like structures were obtained under different Aloe Vera gel concentrations. • The prepared powders were studied for their structural, morphological and luminescence properties. • The observed values indicate that, present powders are effectively used in the fabrication of wLED applications. A multicolored LED illumination device is a compact, durable, easy to obtain color-adjustable output illumination source. It is frequently utilized in the domains of room illumination and exterior displays. However, the advancement of multicolor LEDs has been hampered by the rise in price and the fall in luminous efficacy while changing illumination colors. In the present investigation we have prepared intense red emitting Eu3+ doped CaMoO 4 phosphor nanopowders via simple solid-state reaction technique. The powder X-ray diffraction (PXRD) studies reveal the crystalline nature of the samples with scheelite–type mono phase tetragonal structure with I4 1/a space group. The band gap (E g) energy values were estimated and found to range between 4.63–5.32 eV. Scanning electron microscopy (SEM) studies reveled the hexagonal rod-like structures with different Aloe Vera gel concentrations. The particle size was found to be around 40 nm. The vibrational modes of the prepared powders were evaluated by using Fourier Transform Infrared Spectroscopy (FTIR) and Raman spectroscopy. It was observed from the results that, there were 26 vibrational modes of CaMoO 4 (Γ=3A g + 5A u + 5B g + 3B u + 5E g + 5E u) 8 of which (4A u and 4E u) were infrared active and 13 (A g , B g , and E g) are Raman active. Photoluminescence (PL) emission intensity increases up to 5 mol% of Eu3+ ions load and subsequently it declines due to the concentration quenching phenomenon and effective energy transfer from Mo-O charge transfer band (CTB) to 5D 0 levels of Eu3+. It was noticed from PL emission spectra that, four intense peaks located at 5D 0 → 7F 1 (590 nm), 5D 0 → 7F 2 (613 nm), 5D 0 → 7F 3 (654 nm), 5D 0 → 7F 4 (702 nm) of Eu3+ respectively. The Commission International de I'Eclairage (CIE) diagram indicates the red color emission and average correlated color temperature (CCT) value was found to be 2050 K. Further, the external quantum efficiency (QE) and color purity (CP) were calculated to check the phosphor efficiency and found to be 92% and 72% respectively. The present investigation opens up a new avenue in the fabrication of low-cost display devices with high color purity and luminous efficacy. [Display omitted] [ABSTRACT FROM AUTHOR]

• Aqueous solvation significantly influences the geometric and electronic parameters of diclofenac. • The diclofenac exhibits selective intermolecular hydrogen bonding, primarily with the atom O of group carbonyl and H of group hydroxyl. • Certain hydrogen bonds in diclofenac demonstrate prolonged mean residence times, indicating strong interactions. • Hydrogen bonds in diclofenac -water interactions vary in strength, with some approaching covalent bond characteristics. • Intramolecular NH⋯OH and NH⋯Cl hydrogen bonds crucially affect DDEA's crystal growth and solubility. Diclofenac, a widely used non-steroidal anti-inflammatory drug with analgesic, anti-inflammatory, and antipyretic properties, presents a challenge in oral administration due to its low aqueous solubility and subsequent low bioavailability. This issue, primarily attributed to the drug's high hydrophobicity, can lead to adverse side effects. To address this, our study delves into the aqueous solvation process of diclofenac through molecular modeling, employing both Carr-Parrinello molecular dynamics and Density Functional Theory. This combined approach enables a comprehensive investigation of the molecular interactions that influence solubility, encompassing non-polar interactions (van der Waals dispersion forces), dipole interactions, and hydrogen bonding. Our results highlight the formation of intermolecular interactions with water molecules through OH⋯O water and CO⋯H water hydrogen bonds. Additionally, we observe intramolecular hydrogen bonds within diclofenac (NH⋯OH and NH⋯Cl) and weaker interactions involving CH⋯Cl. Notably, the protonation of diclofenac contributes to molecular rigidity, hindering hydrogen bonding with adjacent water molecules further. These insights offer a deeper understanding of the solubility challenges associated with diclofenac, paving the way for improved drug formulations that enhance bioavailability. The application of Carr-Parrinello molecular dynamics and density functional theory in this study highlights their valuable role in addressing complex drug solubility and design issues. [ABSTRACT FROM AUTHOR]

This study aims to present the hydro-catalytic treatment of organoamine boranes for efficient thermal dehydrogenation for hydrogen production. Organoamine boranes, methylamine borane (MeAB), and ethane 1,2 diamine borane (EDAB), known as ammonia borane (AB) carbon derivatives, are synthesized to be used as a solid-state hydrogen storage medium. Thermal dehydrogenation of MeAB and EDAB is performed at 80 °C, 100 °C, and 120 °C under different conditions (self, catalytic, and hydro-catalytic) for hydrogen production and compared with AB. For this purpose, a cobalt-doped activated carbon (Co-AC) catalyst is fabricated. The physicochemical properties of Co-AC catalyst is investigated by well-known techniques such as ATR/FT-IR, XRD, XPS, ICP-MS, BET, and TEM. The synthesized Co-AC catalyst obtained in nano CoOOH structure (20 nm, 12% Co wt) is formed and well-dispersed on the activated carbon support. It has indicated that Co-AC exhibits efficient catalytic activity towards organoamine boranes thermal dehydrogenation. Hydrogen release tests show that hydro-catalytic treatment improves the thermal dehydrogenation kinetics of neat MeAB, EDAB, and AB. Co-AC catalyzed hydro-treatment for thermal dehydrogenation of MeAB and EDAB acceleras the hydrogen release from 0.13 mL H 2 /min to 46.12 mL H 2 /min, from 0.16 mL H 2 /min to 38.06 mL H 2 /min, respectively at 80 °C. Moreover, hydro-catalytic treatment significantly lowers the H 2 release barrier of organoamine boranes thermal dehydrogenation, from 110 kJ/mol to 19 kJ/mol for MeAB and 130 kJ/mol to 21 kJ/mol for EDAB. In conclusion, hydro and catalytic treatment presents remarkable synergistic effect in thermal dehydrogenation and improves the hydrogen release kinetics. [Display omitted] • Organoamine boranes are synthesis for hydrogen production. • Hydro-catalytic treatment is figure out. • A cobalt doped activated carbon (Co-AC) catalyst is fabricated. • Nano CoOOH structure (20 nm, 12% Co wt) is formed and well-dispersed. [ABSTRACT FROM AUTHOR]

The π-conjugated domain, which is one of frequently-suggested fluorescence origin of carbon dots (CDs), can also act as fluorescence quenching origin in aggregated state. This dual role of the π-conjugated domain in CDs offers a challenge to prediction of photoluminescence (PL) characteristics in solid-state. Here, we focus on the effect of π-conjugated domain on the PL phenomenon for different interparticle separation using three types of CDs with different degree of carbonization. The degree of carbonization was controlled by selecting three alcoholic solvent species for solvothermal reaction, which can influence carbonization of CDs. In dilute dispersion, CDs from three different solvents possessed two emissive centers originated from surface- and core-state with different relative intensities depending on the degree of carbonization. With the increase in concentration of CDs, the higher contents of π-conjugated domain changed the dominant PL center from surface- to core-state due to the greater reduction of surface-derived emission. In aggregated state, the emission from surface-state was totally suppressed, and the π-conjugated domain contents influenced the emission efficiency of core-state. Based on PL decay results, we proposed the PL mechanism of the CDs for different interparticle separation, which would extend the boundary in the interpretation of PL properties of CDs. [Display omitted] • Content of π-domain in carbon dots (CDs) was regulated by changing solvent for the reaction. • In dilute dispersion, π-conjugated domain in the CDs acted as emissive origin. • In concentrated dispersion and solid-state, π-domain accelerated fluorescence quenching. [ABSTRACT FROM AUTHOR]

• Benchmark comparison of Geant4 and MCNP6 in characterisation of fast neutron beam. • SOI Bridge microdosimeter measured experimentally and compared with the two codes. • Neutron capture products from p+ B-implanted regions of the Bridge was investigated. In this study, Monte Carlo codes, Geant4 and MCNP6, were used to characterize the fast neutron therapeutic beam produced at iThemba LABS in South Africa. Experimental and simulation results were compared using the latest generation of Silicon on Insulator (SOI) microdosimeters from the Centre for Medical Radiation Physics (CMRP). Geant4 and MCNP6 were able to successfully model the neutron gantry and simulate the expected neutron energy spectrum produced from the reaction by protons bombarding a 9Be target. The neutron beam was simulated in a water phantom and its characteristics recorded by the silicon microdosimeters; bare and covered by a 10B enriched boron carbide converter, at different positions. The microdosimetric quantities calculated using Geant4 and MCNP6 are in agreement with experimental measurements. The thermal neutron sensitivity and production of 10B capture products in the p+ boron-implanted dopant regions of the Bridge microdosimeter is investigated. The obtained results are useful for the future development of dedicated SOI microdosimeters for Boron Neutron Capture Therapy (BNCT). This paper provides a benchmark comparison of Geant4 and MCNP6 capabilities in the context of further applications of these codes for neutron microdosimetry. [ABSTRACT FROM AUTHOR]

This study demonstrates scalable mechanochemical synthesis of rhodostannite Cu 2 FeSn 3 S 8 nanocrystals. On the contrary to the previous reports focused on the synthesis of stannite Cu 2 FeSnS 4 reporting the rhodostannite impurity, we succeeded in preparing stannite-free product after milling. Pure elements were used for a solvent-free production in a batch of 100 g using an eccentric vibratory mill. The progress of the synthesis was monitored by X-ray diffraction and magnetometry, which both confirmed a successful reaction progress until 6 h of milling. However, further treatment (until 10 h) did not result in an improvement, as quite a high saturation magnetization (7.8 emu/g) and clearly evident diffraction at around 44° in the XRD pattern of the product due to the presence of ferromagnetic un-reacted iron with content slightly above 5% was evidenced. The product is sulfur- and tin-deficient, with crystallite size of around 12 nm. In-depth SEM/EDS analysis has shown the inhomogeneity of Fe distribution due to unfinished reaction. The bandgap of the produced material was 1.29 eV. The spark plasma sintering treatment resulted in complete consumption of non-reacted iron, but partial decomposition to stannite Cu 2 FeSnS 4 was observed. The product is an intrinsic semiconductor with high electrical resistivity, and is therefore unsuitable for thermoelectric application. However, its thermal conductivity is low, thus it could be used as an electrically and thermally insulating material. [Display omitted] • Rhodostannite Cu 2 FeSn 3 S 8 nanocrystals have been successfully produced. • Environmentally friendly solid-state mechanochemical approach has been used. • Scalability of the synthesis up to 100 g per batch was demonstrated. • The product showed interesting electrical and thermal insulating properties. [ABSTRACT FROM AUTHOR]

Nano-sized La–Fe–O (LFO) structures were fabricated via novel free-solvent and green solid-state route using La (acac) 3. H 2 O and Fe (acac) 3 complex precursors. Acetylacetonate (acac) in organometallic complex precursors control nucleation and growth of formed crystals with creation spatial barrier around the cations, and prevent nano-product agglomeration. The mechanism of role of acac has been explained in nanostructure formation. Changing of parameters in synthesis reaction consisting La:Fe molar ratio, calcination time and temperature in turn offer a virtuous control over the nanocomposites size and shape which various compositions of La 2 O 3 /LaFeO 3 , LaFeO 3 /La 2 O 3 and LaFeO 3 /Fe 2 O 3 obtained. The as-prepared La–Fe–O nano-products were characterized thorough Scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), Fourier transform infrared (FT-IR), UV–Vis, BET and energy dispersive X-ray (EDX) analysis in terms of crystallinity structure, composition, porosity and morphology. Different formed La–Fe–O nanostructures were evaluated for electrochemical hydrogen storage capacity through chronopotentiometry technique in stable current (1 mA). The achieved La–Fe–O nanoparticles could be applied as a favorable candidate active material for electrochemical hydrogen storage. Optical, magnetic and reducible characteristics of La–Fe–O nanostructures have positive effect on electrochemical hydrogen storage capacity. It was found out that the LaFeO 3 /Fe 2 O 3 nanocomposites have the best electrochemical hydrogen storage performance due to oxidation-reduction process of Fe2+/Fe3+ components which can help to charge-discharge process of hydrogen to increase the storage capability to 790 mAhg−1 after 20 cycles. Also, the mixed metal oxides illustrate advanced discharge capacity than other binary oxides. • Synthesis of La–Fe–O nanocomposites via cost-effective solid-state technique. • Investigation of divers synthesis circumstances on dimension properties of nanostructures. • Consideration of electrochemical hydrogen storage capacity of obtained nanostructures. • Discharge efficiency of 790 mAhg−1 after 20 cycles for LaFeO 3 /Fe 2 O 3 nanocomposites. [ABSTRACT FROM AUTHOR]

For the first time, we report the Li-ion storage performance of V 10 O 24.nH 2 O with LiPF 6 based liquid electrolyte (LE) and PDATFSI-60IL based solid-polymer electrolyte (SPE). The LiǁV 10 O 24.nH 2 O in LE exhibits a reversible capacity of ∼184/83 mAh g−1 at 0.1/5.0 A g−1, respectively, and features good cycling stability (retained 98.78, and 65.53 % after 1000 and 2000 cycles, respectively). In case of solid-state Li-ion battery (ssLiB), the PDATFSI-60IL membrane is utilized as SPE as well as binder for V 10 O 24.nH 2 O cathode material. The PDATFSI-based SPE effectively provides reliable Li+ conductive galleries, prevents the Li dendrites formation, and provides stable contact between the cathode and current collector. The resultant V 10 O 24.nH 2 O cathode exhibit a reversible capacity of ∼152 mAh g−1 at 0.1 A g−1, demonstrating good rate performance (≈152/38 mAh g−1 at 0.1/5 A g−1) with considerable cycling stability (≈72 % capacity retention at 500th charge/discharge cycle). We report Li-ion storage performance of V 10 O 24.nH 2 O with LiPF 6 based liquid electrolyte (LE) and PDATFSI-60IL based solid-polymer electrolyte (SPE). The PDATFSI-60IL membrane is utilized as SPE as well as binder for V 10 O 24.nH 2 O cathode material. [Display omitted] • PDATFSI is used as both SPE and binder for LiǁV 10 O 24.nH 2 O battery. • LiǁV 10 O 24.nH 2 O exhibit ∼184/83 mAh g−1 at 0.1/5 A g−1, respectively. • In ssLIB, LiǁV 10 O 24.nH 2 O exhibit 152/38 mAh g−1 at 0.1/5 A g−1, respectively. • V 10 O 24.nH 2 O exhibits dominant pseudocapacitive charge storage mechanism. • V 10 O 24.nH 2 O exhibits low-self discharge properties in both liquid and SPE. [ABSTRACT FROM AUTHOR]

In this study, an innovative self-supporting electrolyte has been prepared and applied to electrochromic device with a structure of ITO/WO 3 /SSE/NiO/ITO. Since the self-supporting electrolyte exhibits excellent transparency and high ionic conductivity, enabling the electrochromic device to demonstrate superior electro-optical performance including: a significant optical transmittance modulation (41.2 % at 550 nm), good cycling stability (retaining 95 % optical transmittance modulation at 550 nm after 1000 cycles), and high coloration efficiency (87 cm2 C⁻1 at 550 nm). Taking into account the easy preparation characteristics of this electrolyte and its suitability for large-scale device preparation, it can be considered as a potential candidate for electrolytes applied in high-performance electrochromic devices in the future. Solid-state ECD based on the SSE exhibits good electro-optical properties. [Display omitted] • Self-supporting electrolyte has been prepared by solution photoinitiated polymerization method. • Self-supporting electrolyte exhibits high transparency and a good ionic conductivity of 1.8*10−5 S cm−1. • Electrochromic device based on self-supporting electrolyte displays excellent electro-optical performance. • Electrochromic device based on self-supporting electrolyte shows a high coloration efficiency of 87 cm2 C⁻1 at 550 nm. [ABSTRACT FROM AUTHOR]

Buccal matrices represent a widely accepted dosage form permitting a convenient, easy, reliable drug administration and reducing administration errors. The aim of this study was the development of mucoadhesive buccal matrices for propranolol administration in children. Matrices were obtained by freeze-drying of drug loaded polymeric solutions based on gum tragacanth (GT), pectin (PEC), hydroxypropylmethylcellulose (HPMC), sodium hyaluronate (HA), gelatin (GEL), chitosan (CH) or a mixture of CH and HPMC (CH/HPMC). Matrices were characterized for drug solid state, morphology, water-uptake, mucoadhesion ability, in vitro drug release and permeation through porcine epithelium. The most promising formulations were tested for in vitro biocompatibility in human dental pulp fibroblasts. The preparative method and the polymeric composition influenced the drug solid state, as a complete amorphization as well as different polymorphic forms were observed. GEL and PEC guaranteed a fast and complete drug release due to their rapid dissolution, while for the other matrices the release was influenced by drug diffusion through the viscous gelled matrix. Moreover, matrices based on CH and CH/HPMC showed the best mucoadhesive properties, favoured the drug permeation, in virtue of CH ability to interfere with the lipid organization of biological membrane, and were characterized by a good biocompatibility profile. [ABSTRACT FROM AUTHOR]

The Methanation of CO 2 to CH 4 is a significant route to save energy and reduce CO 2 emission. In this work, a series of Cr 2 O 3 –Al 2 O 3 powders were synthesized by a novel and simple solid-state method and considered as the carrier for the nickel catalysts in CO 2 methanation. The BET area and pore volume of the supports decreased with the decrease in Al 2 O 3 /Cr 2 O 3 molar ratio. The results indicated that the increase in Cr 2 O 3 content improved the catalytic performance and 15 wt%Ni/Cr 2 O 3 catalyst exhibited the highest CO 2 conversion of 80.51%, and 100% CH 4 selectivity at 350 °C. The results indicated that the CO 2 conversion improved with the increment in H 2 /CO 2 molar ratio from 2 to 5. The improvement in CO 2 conversion was also observed with decreasing GHSV due to the longer residence time of the reactants on the catalyst surface. Also, the results showed that increasing calcination temperature led to a decrease in CO 2 conversion. The 15 wt%Ni/Cr 2 O 3 catalyst exhibited high stability in carbon dioxide methanation reaction. • BET area decreased with increasing Cr 2 O 3 content in Cr 2 O 3 –Al 2 O 3 carrier. • The activity in CO 2 methanation depends on the reducibility of nickel species. • Ni/Cr 2 O 3 showed the highest methanation activity, CH 4 selectivity and stability. • The Cr 2 O 3 –Al 2 O 3 supports were prepared using a facile solid-state method. [ABSTRACT FROM AUTHOR]

We report in this communication a ready-to-use fused deposition modeling (FDM) based 3D-printed spectroelectrochemical cell to perform for the first time voltammetry of immobilized microparticles (VIMP) and Raman spectroscopy in situ using acrylonitrile butadiene styrene (ABS) as the filament material for printing. The 3D-printed cell was applied to evaluate solid state electrochemical behavior of tadalafil as a proof-of-concept. Several advantages were achieved in the use of the developed device, such as less manipulation of the working electrode, monitoring the same region of the solid microparticles before and after electrochemical measurements, better control of the laser incidence, low-cost and low-time production. Furthermore, the device was printed in a single-step, without handling to assembly and it has an estimated material cost of approximately 2 $. The use of 3D-printing technology was significantly important to integrate Raman spectroscopic method with VIMP measurements and to support mechanism elucidation and characterization of the compounds with less manipulation of the working electrode, avoiding loss of solid products formed from electrochemical reactions. Image 1 • 3D-printed spectroelectrochemical cell for coupling voltammetry of immobilized microparticles and Raman spectroscopy. • Possibility of in situ measurements without manipulation of the working electrode. • Single-step printing using FDM printer, low-cost and low-time production of the cell. • Better visualization of the changes in Raman spectra during solid-state electrochemical measurements. [ABSTRACT FROM AUTHOR]

Four forms of a salt combining two antitubercular drugs, clofazimine and 4-aminosalicylic acid, are reported and the crystal structure of two of these forms are described. TG/DSC analysis of all four forms demonstrate an increase in the temperature at which degradation (upon decarboxylation) occurs in comparison to pure 4-aminosalicylic acid. Water solubility evaluation indicates a significant increase of the amount of clofazimine detected in water (10.26 ± 0.52 μg/mL for form I, 12.27 ± 0.32 μg/mL for form II, 7.15 ± 0.43 μg/mL for form III and 8.50 ± 1.24 μg/mL for form IV) in comparison to pure clofazimine (0.20 ± 0.03 μg/mL). [ABSTRACT FROM AUTHOR]

All-solid-state rechargeable Zn-air battery is deemed to be a promising class of power source for its attractive operational safety and mechanical flexibility. To achieve high performance of Zn-air battery, the density of active sites on the ORR/OER bifunctional electrocatalyst and the maximized access to them are of great importance. In this study, a nitrogen, sulfur and ferric co-doped three-dimensional bifunctional catalyst (FeN x /N,S–C) is developed via a facile and eco-friendly molten salt assisted synthesis. The homogeneously dispersed FeN x species, the surrounding S dopants and the 3D hierarchical architecture synergistically endow FeN x /N,S–C with dense active sites with high accessibility, abundant open pores/channels and efficient mass transfer. Compared with the commercial Pt/C–RuO 2 catalyst, the application of FeN x /N,S–C in all-solid-state rechargeable Zn-air batteries results in enhanced ORR/OER activities, lower charge-discharge voltage gaps and improved 52 h cycling durability, implying its good feasibility in practical application. The all-solid-state FeN x /N,S–C based battery shows no performance decay during charge-discharge cycles when its sodium polyacrylate hydrogel electrolyte is compressed up to 67% strain or stretched up to 400% length, implying the feasibility of the present FeN x /N,S–C catalyst in the usage of stable and flexible electronics. Image 1 [ABSTRACT FROM AUTHOR]

In this work, the BaAl2O4: Eu2+, Eu2+/L3+ (L= Dy, Er, Sm, Gd, Nd, and Pr) phosphors were synthesized via a facile solid-state reaction method using LiCl as a flux material at 1100 °C. The structural properties, microstructure, adsorption and photoluminescence characteristics of products were evaluated by X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Uv–vis adsorption and photoluminescence (PL) analyses. The observation of XRD patterns showed that even 10% LiCl is not able to produce any impurity phase in BaAl 2 O 4 : Eu2+ crystal structure, although the microstructure morphology is considerably affected. The particle size of BaAl 2 O 4 : Eu2+ phosphors was about 220 nm while the use of LiCl flux resulted in a remarkable decrease of this parameter to about 120 nm. Furthermore, the PL patterns disclosed that Eu2+ ions have occupied one type of Ba2+ sites while larger quantities of lanthanides (L3+) occupied the second type of Ba2+ sites. The strongest photoluminescence emission intensity at the wavelength of 495 nm was achieved when 5 wt% LiCl was added to BaAl 2 O 4 : Eu2+. Also, the absorption analysis revealed that the addition of flux enriches the adsorption of Congo red (CR) dye on the phosphor powders. The use of 5 wt% flux material led to noticeable improvement of CR adsorption capacity from 38.53 to 48.3 mg g−1. [ABSTRACT FROM AUTHOR]

We sought to demonstrate the usefulness of the T 2 relaxation behaviors measured by time domain NMR (TD-NMR) for the quantitative evaluation of the crystallinity of an active pharmaceutical ingredient (API). This study used indomethacin as a model API. After blending amorphous and crystalline indomethacin powders at a designated ratio, T 2 relaxation curves were measured by TD-NMR. Subsequently, we acquired a calibration curve to quantify crystallinity by curve fitting analysis. Validation demonstrated a good correlation between the theoretical and experimental percentage of crystallinity. Thus, this study succeeded in a precise estimation of crystallinity of indomethacin using TD-NMR. We also investigated whether the technique is practical by testing indomethacin powders with unknown proportion of crystallinity, and then compared their estimated crystallinity with that found using conventional evaluation techniques. The quantitative performance of the TD-NMR technique was comparable to that of Raman spectroscopy. Furthermore, indomethacin powder blended with excipients, which can be used to produce tablets, was tested. The TD-NMR technique was still able to quantify the crystallinity of indomethacin, even when excipients were incorporated into the sample. Therefore, the present study expands the horizon for evaluating the crystallinity of APIs in pharmaceutical sciences. [ABSTRACT FROM AUTHOR]

A biopharmaceutics classification system class IV drug, hydrochlorothiazide (HCT), was combined with co-formers of L-and d -arginine (ARG) and sodium lauryl sulphate (SLS) by cryomilling in 1:1 molar ratio. Co-amorphization was observed with L- and D-ARG. These mixtures showed a single glass transition, evidence of possible salt formation and improved physical stability at elevated temperatures and/or humidity when compared with amorphous HCT. The co-amorphous formulations, along with the combinations of HCT and HCT:L-ARG with polyvinylpyrrolidone (PVP) in 1:1 mass ratio, were investigated with a simultaneous dissolution/permeation setup using parallel artificial membrane permeability assay (PAMPA) or Madine Darby kidney cells (MDCKII) as the permeation barrier. It was observed that co-amorphization with L-ARG and D-ARG was able to induce a supersaturated state for HCT, possibly through intermolecular interactions, but there was virtually no difference between the dissolution properties of the mixtures formed with the 2 optical isomers of ARG. The permeability of HCT was found to be dependent on the dissolution properties of the formulations in both PAMPA and cellular barrier experiments. Thus, co-amorphization of HCT with L- and D-ARG demonstrated the possibility to enhance the dissolution and thereby the permeation potential of a BCS class IV drug. [ABSTRACT FROM AUTHOR]

The application of hot melt coating (HMC) as an economic and solvent-free technology is restricted in pharmaceutical development, due to the instable solid-state of HMC excipients resulting in drug release instability. We have previously introduced polyglycerol esters of fatty acids (PGFAs) with stable solid-state (Part 1). In this work we showed a novel application of PGFAs as HMC excipients with stable performance. Three PGFA compounds with a HLB range of 5.1–6.2 were selected for developing immediate-release formulations. The HMC properties were investigated. The viscosity of molten lipids at 100 °C was suitable for atomizing. The DSC data showed the absence of low solidification fractions, thus reduced risk of agglomeration during the coating process. The driving force for crystallization of selected compounds was lower and the heat flow exotherms were broader compared to conventional HMC formulations, indicating a lower energy barrier for nucleation and lower crystallization rate. Lower spray rates and a process temperature close to solidification temperature were desired to provide homogeneous coating. DSC and X-ray diffraction data revealed stable solid state during 6 months storage at 40 °C. API release was directly proportional to HLB and indirectly proportional to crystalline network density and was stable during investigated 3 months. Cytotoxicity was assessed by dehydrogenase activity and no in vitro cytotoxic effect was observed. [ABSTRACT FROM AUTHOR]

Successful development of stable solid protein formulations usually requires the addition of one or several excipients to achieve optimal stability. In these products, there is a potential risk of an inhomogeneous distribution of the various ingredients, specifically the ratio of protein and stabilizer may vary. Such inhomogeneity can be detrimental for stability but is mostly neglected in literature. In the past, it was challenging to analyze inhomogeneous component distribution, but recent advances in analytical techniques have revealed new options to investigate this phenomenon. This paper aims to review fundamental aspects of the inhomogeneous distribution of components of freeze-dried and spray-dried protein formulations. Four key topics will be presented and discussed, including the sources of component inhomogeneity, its consequences on protein stability, the analytical methods to reveal component inhomogeneity, and possible solutions to prevent or mitigate inhomogeneity. [ABSTRACT FROM AUTHOR]

Excipients used in lyophilized protein drug products are often selected by a trial-and-error method, in part, because the analytical methods used to detect protein-excipient interactions in lyophilized solids are limited. In this study, photolytic labeling was used to probe interactions between salmon calcitonin (sCT) and excipients in lyophilized solids. Two diazirine-derived photo-excipients, photo-leucine (pLeu) and photo-glucosamine (pGlcN), were incorporated into lyophilized solids containing sCT, together with an unlabeled excipient (sucrose or histidine) at prelyophilization pH values from 6 to 9.9. Commercially available pLeu was selected as an ionizable photo-excipient and amino acid analog, while pGlcN was synthesized as an analog of sugar-based excipients. Photolytic labeling was induced by exposing the solids to UV light (365 nm, 30-60 min), and the resulting products were identified and quantified with liquid-chromatography mass spectrometry. The distribution of photo-reaction products was affected by the photoreactive reagent used, the type of unlabeled excipient, and the solution pH before lyophilization. When other components of the solid were identical, the extent and sites of labeling on sCT were different for pGlcN and pLeu. The results suggest that ionizable and nonionizable excipients interact differently with sCT in lyophilized solids and that photo-excipients can be used to map these interactions. [ABSTRACT FROM AUTHOR]

Low-cost multi-heteroatom doped porous carbons derived from agricultural waste were prepared as the base material. Then, the cobalt oxides nanosheets were anchored to the surface of the carbon material to obtain the composites. It was found that the adoption of porous carbon is of great significance for the improvement of materials properties. The presence of porous structure derived from carbon materials not only increases the stability of the material, but also facilitates the diffusion and transfer of electrolyte ions. Meanwhile, the flaky Co 3 O 4 endows the material with high energy density and high charge transport efficiency. The resulted composite materials exhibit high specific surface area with low electrochemical impedance. Both aqueous and solid-state SCs were assembled separately. The energy density of aqueous SC can reach up to 42.5 Wh kg−1 at a power density of 746 W kg−1 and even with power density up to 30 kW kg−1 as the energy density still maintained 25 Wh kg−1. As for solid-state SC, the energy density can reach 40.6 μWh cm−2. The retention of solid-state SC can maintain at 87.1% even after 3000 cycle numbers. The excellent performance of composites enables them to be promising electrode materials for energy storage. Image 1 [ABSTRACT FROM AUTHOR]

In this research YVO 4 :Dy 3+ luminescent material was synthesized via a facile and one-step solid state method at 1100 °C. Then the effects of spherical and irregular SiO 2 particles on microstructure and photoluminescence properties of the phosphors were investigated in details. To study about the microstructure and characteristics of these composites, XRD, SEM, TEM, HRTEM, XPS and PL equipment were employed. The XPS results proved that via the addition of SiO 2 , strong bonding is produced between SiO 2 particles and YVO 4 :Dy3+ phosphors and based on the stronger electronegativity of Si 2p compared to Y 3d and V 2p elements, the increase of binding energy has occurred. Moreover, this research showed that the addition of 7 wt% spherical SiO 2 particles provides strongest excitation and emission luminescence properties. Interestingly, further increase of SiO 2 results in the suppression of emission intensity. Also, it was found that the emission intensities of the phosphors including SiO 2 spheres are significantly stronger than the phosphors consisting irregular shape SiO 2 which can be interpreted by the light scattering phenomenon. Via finite difference time domain (FDTD) simulation, it was revealed that the scattering cross section of the phosphors consisting spherical SiO 2 is significantly smaller than that of the phosphors consisting irregular SiO 2. In addition, the reflection of the former is less than that of the latter since SiO 2 spheres cover more empty spaces among YVO 4 particles. [ABSTRACT FROM AUTHOR]

[Display omitted] Mebendazole (MBZ) is a broad-spectrum active pharmaceutical ingredient (API) indicated for treating parasitosis, and it has three solid-state forms, A, B, and C. These solid forms exhibit significant differences in dissolution properties, which cause considerable changes in the therapeutic effect. When at least 30 % of Form A is present in the formulation, it has a similar effect to the placebo. The aim of this study was to develop a reliable quantitative method for MBZ (Forms A and C) suspensions that allowed to study the solid-state stability and the kinetics of the solid-state transformation of MBZ suspensions under the recommended pharmaceutical industry conditions. One method was developed to carry out the drying process and the other one to quantify Forms A and C of MBZ suspensions; both were evaluated. For the stability study, samples were prepared with different starting reference concentrations of Form A and stored from 1 to 24 months under long-term stability conditions (30 ± 2 °C and 75 ± 5 % RH) and from 1 to 6 months under accelerated stability conditions (40 ± 2 °C and 75 ± 5 % RH). Data collection was performed by powder X-ray diffraction (PXRD). The Rietveld method (RM) and Topas's program were used to solid form quantification. Avrami's equation was used to determine the kinetic parameters. The results showed that the combination of the drying process and solid form quantification developed method for suspension was a very accurate methodology for solid-state stability studies. Furthermore, in long-term and accelerated solid-state conditions, suspension with an initial value of 1 % of Form A were sufficient to cause a solid-state transformation (Form C to A) greater than 30 % in the first and second months, with a complete transformation in nine and six months respectively. These results demonstrate that suspensions show complete solid-state transformation (Form C to A) in a shorter time than the product's shelf life (∼2 years). In this work, a reliable methodology was developed to quantify MBZ (Forms A and C) suspensions. This methodology could be used to control the different solid forms for MBZ and other APIs to avoid solid-state transformation problems. [ABSTRACT FROM AUTHOR]

Red-emissive carbon dots (R-CDs), as a novel type of carbon nanomaterial, have attracted extensive attention in various fields due to their unique properties and physicochemical characteristics. However, most of the reported R-CDs have mainly shown fluorescence in solution, which seriously limits their practical applications, especially in anticounterfeiting and optoelectronic device fields. In recent years, significant efforts have been devoted to achieving solid-state red fluorescence of CDs and exploring their potential applications. In this review, we analyzed the key issues in the synthesis of solid-state red carbon dots (SSR-CDs), elucidated the possible mechanisms of anti-quenching, and introduced their applications. Finally, we discuss the current challenges and opportunities of SSR-CDs. • We summarize the existing research and emerging advances of such CDs from a particular angle to guide their synthesis with desirable optical properties. • We focus on their solid-state fluorescent (SSF) mechanism from the molecular structure design to achieve AIE, R-CDs in such a solid-state matrix and CEE. • The applications of SSR-CDs, especially in photoelectric device applications and anti-counterfeiting applications, are summarized to determine their potential value. [ABSTRACT FROM AUTHOR]

This study investigates the correlation between the structural and release properties of solid lipid microparticles (MPs) of tristearin containing 5 % w/w of four different liquid additives used as crystal modifiers: isopropyl myristate (IM), ethyl oleate (EO), oleic acid (OA) and medium chain triglycerides (MCT). All additives accelerated the conversion of the unstable α-form of tristearin, formed after the MPs manufacturing, to the stable β-polymorph and the transformation was completed within 24 h (for IM and EO) or 48 h (for OA and MCT). The kinetic of polymorphic transition at 25 °C was investigated by simultaneous synchrotron SAXS/WAXS and DSC analysis after melting and subsequent cooling of the lipid mixture. After crystallization in the α-phase, additives accelerate the solid-solid phase transformation to β-tristearin. SAXS data showed that two types of structural modifications occurred on MPs during storage: compaction of the crystal packing (slight decrease in lamellar thickness) and crystal growth (increased number of stacked lipid lamellae). The release behavior of a model hydrophilic drug (caffeine) at two different amounts (15 % and 30 %) from MPs was studied in water and biorelevant media simulated the gastric and intestinal environment. It was particularly significant that the introduction of IM, EO and MCT were able to prolong the drug release in water, passing from a diffusion-based Higuchi kinetics to a perfect zero-order kinetic. Moreover, the overall release profiles were higher in biorelevant media, where erosion/digestion of MPs was observed. After 6 months, a moderate but statistically significant change in release profile was observed for the MPs with IM and EO, which can be correlated with the time-dependent structural alterations (i.e. larger average crystallite size) of these formulations; while MPs with OA or MCT displayed stable release profiles. These findings help to understand the correlation between release behavior, polymorphism and supramolecular‐level structural modification of lipid formulations containing crystal modifiers. [Display omitted] [ABSTRACT FROM AUTHOR]

[Display omitted] Olivine lithium manganese phosphate was synthesized by a mechanochemical method. Inorganic cathode materials can be divided into three kinds of lithium metal oxide layered, spinel oxide and olivine metal phosphate. One important of the cathode materials used in Li-ion cells is LiMnPO 4. In this paper two different precursors, manganese violet and ammonium manganese phosphate proposed as reactant in the synthesis of LiMnPO 4 nanostructures. Reaction between NH 4 MnP 2 O 7 and Li 2 CO 3 takes placed in solid state at room temperature. In this mechanochemical process, a solid acid and base reaction occurred between ammonium and carbonate ions. In addition, MnIII is unstable oxidation state and convert to crystalline β-MnO 2 , Li 2 MnP 2 O 7 and NH 4 H 2 PO 4 in the disproportionation reaction. Results showed that mechanochemical reaction between NH 4 MnP 2 O 7 with Li 2 CO 3 as precursors lead to concurrent redox and acid-base reaction. As a result, we observed there is a tendency for manganese violet to disproportionation into MnO 2 and manganese pyrophosphate salt in a solid-state reaction. Finally, a redox reaction between β-MnO 2 and Li 2 MnP 2 O 7 in pyrolysis reaction under inert atmosphere give LiMnPO 4. In the other hand in the mechanochemical reaction between NH 4 MnPO 4 and Li 2 CO 3, only acid and base reaction occurred and the NH 4 + ions were replaced with Li+ ions and amorphous LiMnPO 4 was prepared. The amorphous LiMnPO 4 convert to crystalline LiMnPO 4 by annealing the powder under inert atmosphere. The chemical changes in formation of LiMnPO 4 compound was characterized by X-Ray diffraction analysis (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and energy dispersion x-ray analyses (EDX). FTIR spectra showed that the NH 4 + ions were replaced with Li+ ions. X-ray diffraction show that by variation of precursor from manganese violet to ammonium manganese phosphate in the mechanochemical reaction the crystalline pattern changes to amorphous and also the reaction pathway was changed. The SEM images of LiMnPO 4 nanoparticles that obtained by two precursors exhibit squamous morphologies with well-defined grain boundaries and nonuniform particle size distributions. The particle size distributions of crystalline LiMnPO 4 obtained by NH 4 MnP 2 O 7 and NH 4 MnPO 4 were found in the region 60–260 and 20–130 nm respectively. [ABSTRACT FROM AUTHOR]

• The x = 0.12 ceramic shows a large W rec and high η at E b of 740 kV/cm. • The x = 0.12 ceramic exhibits a large current density. • The x = 0.12 ceramic exhibits a high power density. • The x = 0.12 ceramic possess excellent temperature stability and fatigue resistance. (1- x)NaNbO 3 - x Bi(Fe 0.5 Sc 0.5)O 3 (NN- x BFS) ceramics were prepared by solid-state sintering method. All samples have pseudocubic structure and micron-sized grains. The addition of BFS promotes the generation of polar nanoregions, maintains large polarization, and enhances the ability to resist external electric fields, creating conditions for achieving high energy storage density W rec and efficiency η simultaneously. The x = 0.12 ceramic shows a high W rec of 4.32 J/cm3 and large η of 85 % at 740 kV/cm, together with excellent power density of 325 MW/cm3, large current density of 1327 A/cm2, ultra fast discharge speed of 64 ns and strong hardness of 3.56 GPa. Good temperature stability in the range of 20 ∼ 160 °C and excellent fatigue resistance under 106 cycles are attained. The findings of this study can help us better perform composition design to promote the collaborative optimization of energy storage density and efficiency of ceramics. [ABSTRACT FROM AUTHOR]

Due to the growing worries about environmental issues, dye degradation is substantial. Besides that, it is essential to prevent illness development by creating cutting-edge antibacterial agents that can inhibit bacterial activities. Herein, we report a novel photocatalyst exhibiting visible light responsivity for the degradation of methyl violet dye and possessing antibacterial properties to mitigating the emergence of drug resistance. It is triple-doped ZnO (Mg, Cu, N-doped ZnO, and Mg, Cu, B-doped ZnO), successfully synthesized by the solid-state method. The structure crystal is hexagonal wurtzite, and the crystal size is 34.68, 30.22, and 29.47 nm for undoped ZnO, (Mg, Cu, N)-doped ZnO, and (Mg, Cu, B)-doped ZnO, respectively, according to the study of X-ray diffraction (XRD), Raman, and SEM results. The (Mg, Cu, N)- and (Mg, Cu, B)-doped ZnO have smaller particle sizes than undoped ZnO. FTIR spectra show Zn-O, Cu-O, Mg-O,and B-O stretching for synthesized samples. The formation of (Mg, Cu, N)-doped ZnO and (Mg, Cu, B)-doped ZnO also were confirmed by EDAX. PL shows the formation of peaks in UV emission (∼350 nm) and visible emission (513–519 nm and ∼646 nm) that indicate the inhibition of electron-hole recombination and oxygen vacancies in the ZnO lattice. The effective photocatalytic activity of undoped ZnO, (Mg, Cu, N)-doped ZnO, and (Mg, Cu, B)-doped ZnO achieves 80.89 %, 93.41 %, and 92.18 % decolorization of water pollutant methyl violet. The antibacterial activities of the three samples are 6.45, 6.00, and 11.90 mm, respectively. [Display omitted] [ABSTRACT FROM AUTHOR]

[Display omitted] • State-of-art for synthesis of tin oxide-based materials towards supercapacitor applications. • Widespread synthetic routes bare SnO 2 , SnO 2 with composite, metal doped, metal doped composites. • Supercapacitors through single electrode, liquid, solid-state, symmetric, asymmetric modes. • Demonstrating of supercapacitor from small scale to advance wearable applications. • Present challenges with future prospects for SnO 2 based materials for supercapacitor. Increased population causing need of efficient energy storage devices possessing high energy density and environmental friendliness. Electrochemical supercapacitor is one who can fulfil the future demands. In this regard, many materials have been synthesized towards low-cost fabrication process to serve as efficient and effective energy storage supercapacitive devices but not up to the mark in wide-spread applications and commercially large-scale production. Tin oxide is cheap, earth abundant, electrically conductive, and a structurally stable material and poses pseudocapacitive behavior. In this regard, present review explores tin oxide-based materials towards active electrode material for supercapacitor applications. Supercapacitors can be classified as electrochemical double layer (EDLC) behaved where charge store at electrode-electrolyte interface possessing high stability but suffers through low capacitance. Contrary, pseudocapacitive through redox reactions possess high capacitance but suffers through low stability. High stability with high capacitance can be achieved through 'material mutualism' between EDLC and pseudocapacitive behaved materials, where tin oxide behaves as a pseudocapacitive material. Hence, critical review explores not only bare tin oxide material but also its composites with carbon-based materials, polymers, metal oxides, metal sulfides, ternary nanocomposites, and it's doping along with composite formation as well. These are well categorised through wide spread synthetic routes such as hydrothermal, chemical precipitations, electrochemical deposition, spray pyrolysis, chemical bath deposition, successive ionic layer adsorption and reaction, electrospinning, sonochemical, atmospheric pressure plasma jet and thermal evaporation from synthesis, characterization to application part. Supercapacitors through single electrode, liquid and solid-state configured symmetric and asymmetric devices have been well explored along with highlights for the future scope inclusive of flexible and wearable devices. [ABSTRACT FROM AUTHOR]

Microwave (MW) ovens, powered by traditional magnetrons, often produce unpredictable heating patterns in foods due to their wide and random frequency spectrum. This study investigated the potential of solid-state (SS) MW generators to overcome this limitation. The frequency spectra of the SS generator were measured, computer simulation and experimental methods were used to analyze the standing wave and heating patterns within foods. The influence of SS operating frequency on MW power reflection and heating uniformity was also examined. The results show that the SS generator's operating frequency bandwidth was less than 0.1 MHz, approximately 1/500th that of magnetrons. This narrow and stable bandwidth enabled the SS-powered cavity to support a single standing wave pattern (mode), resulting in stable and predictable heating patterns in foods. Moreover, adjusting SS operating frequency could minimize MW power reflection, using complementary SS frequencies could improve MW heating uniformity. This study provides fundamental insights into SS MW heating and offers guidance on controlling SS frequency to improve heating performance. • Frequency spectra of a solid-state generator were measured. • Standing wave patterns in a multi-mode cavity were calculated. • Solid-state generators provided a single standing wave pattern. • Solid-state generators provided a predictable and stable heating pattern of foods. • Proper frequency control improved heating uniformity and energy coupling. [ABSTRACT FROM AUTHOR]

[Display omitted] The present study aims to outline a rational framework for the design and development of a 1.0% (w/v) hydrocortisone nanocrystal-based formulation, resorting to a simple, efficient, and scalable nanonization methodology, based on the high-pressure homogenization (HPH) technique. Accordingly, the innovative product was comprehensively optimized following a Quality by Design (QbD) approach. The thorough selection of formulation composition was driven by a dual purpose: improving skin permeation and stability. In the early stage of development, a Failure Mode, Effects and Criticality Analysis (FMECA) diagram was employed to identify the most impactful variables for the critical quality attributes (CQAs). In this sense, a rotatable, three-factor and five-level circumscribed central composite design (CCCD) was applied to investigate how squalene concentration (x 1), soluplus concentration (x 2) and HPH-time (x 3) influence physicochemical properties, performance and physical stability of the formulation. A robust Design Space (DS) was defined, establishing the optimal settings for the critical variables, whose combination meets the requirements set in the quality target product profile (QTPP). Morphological analysis revealed the cuboidal shape of hydrocortisone nanocrystals. In what concerns colloidal properties, the most promising formulation disclosed a small particle size (Dx(50) = 311.8 ± 1.5 nm), along with narrow size distribution (span value = 1.91 ± 0.17). Zeta potential results (−2.19 ± 0.15 mV–−12.1 ± 0.4 mV) suggested a steric hindrance stabilization. FTIR spectra showed no chemical interactions between drug and formulation components. XRD diffractograms confirmed loss of crystallinity during the downsizing process. In vitro studies revealed an improvement on drug release rate (316 ± 21–516 ± 35 μg/cm2/√t), compared to the coarse suspension and commercial products, and a straight dependence on the stabilizer concentration and HPH time. The permeation flux across the skin (0.16 ± 0.02–1.2 ± 0.5 μg/cm2/h) appeared to be dependent on the drug physicochemical properties, in particular saturation solubility. Further characterization of the experimental formulations pointed out the role of the stabilizing component to prevent against physical instability phenomena. This organic solvent-free, and therefore "green" nanocrystal production technology offers great potential for pharmaceutical R&D and drug delivery by enabling the development of new forms of conventional drugs with optimal physicochemical properties and performance. [ABSTRACT FROM AUTHOR]

Co-crystals have received increasing attention during the past decades for their ability to modify the solubility and other physicochemical properties of active pharmaceutical ingredients. Apigenin (Agn) and Daidzein (Dai) are flavonoid compounds with a variety of biological effects. However, the bioavailability and clinical applications of flavonoid compounds are usually limited by their poor aqueous solubilities. In this study, theophylline (Thp) is used as a coformer to co-crystallize with Agn and Dai. The solid-state properties of the co-crystals of Thp with Agn and Dai are characterized by powder X-ray diffraction, thermogravimetric analysis, differential scanning calorimetry, Raman spectroscopy, and nuclear magnetic resonance experiments. In addition, both co-crystals show a greater resistance to hydration than Thp alone. The solubilities, intrinsic dissolution rates, and permeabilities of Agn - Thp co-crystal and Dai - Thp co-crystal are improved compared with those of parent flavonoids. The pharmacokinetic study shows that the bioavailabilities of both co-crystals are enhanced in comparison with the corresponding physical mixtures and parent flavonoids. This study demonstrates that the co-crystallization by using theophylline is a promising strategy to improve physicochemical properties and bioavailability of flavonoid compounds. [ABSTRACT FROM AUTHOR]

Highlights • A theoretical model of intra-cavity pumped dual-wavelength laser which considering reabsorption loss has been introduced. • The theory of intracavity-pumped dual-wavelength laser is feasible, and the error is within the allowable range. • The individual output power for the 912 nm and 1064 nm emissions were 0.43 W and 0.9 W, respectively. • A no gain competition between the 912 nm and 1064 nm transitions is implemented for the first time to our best knowledge. Abstract A dual-wavelength continuous-wave laser with direct intra-cavity pumping using a 879 nm laser diode that utilizes Nd:GdVO 4 and Nd:YVO 4 crystals, is presented. To the best of our knowledge, this system completely eliminates the gain competition between the 912 nm and 1064 nm transitions for the first time. A theoretical model is introduced to describe this intra-cavity pumped dual-wavelength laser. The lasing threshold of the 912 nm Nd:GdVO 4 laser is presented by considering the ground-state reabsorption loss effect. A total output power of 1.33 W at dual-wavelength operation with an absorbed pump power of 7.91 W is experimentally achieved. The individual output power for the 912 nm and 1064 nm emissions were 0.43 W and 0.9 W, respectively. Both wavelengths operate in TEM 00 mode with a total slope efficiency >20%. [ABSTRACT FROM AUTHOR]

Spironolactone (SPR) is a poorly water-soluble drug widely used for the treatment of various diseases. The objective of this study was to carry out the preparation and solid-state characterization of SPR 1/3 hydrate. The solid form was generated by an unreported recrystallization process in acetone and characterized for the first time by a combination of X-ray powder diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), Fourier-transform infrared spectroscopy (FTIR), equilibrium solubility, and an accelerated stability study. XRD, DSC, and TGA studies revealed that SPR 1/3 hydrated converts completely to form II after heating to 180°C. Solubility studies at 37°C showed that SPR 1/3 hydrate was statistically less soluble than SPR form II in all tested media and that SPR form II partially converts to SPR 1/3 hydrate in aqueous media. Accelerated stability studies demonstrated that both forms were physically and chemically stable up to 6 months (40°C/75% RH). We concluded that contamination of SPR 1/3 hydrate in SPR raw materials is undesirable. Taking this into account we recommend its polymorphic monitoring either in active pharmaceutical ingredients or commercial tablets by solid-state identification/quantification methods (XRD, DSC, TGA, and FTIR). Of these, XRD proved to be the most conclusive and accurate. [ABSTRACT FROM AUTHOR]

Abstract Titanium alloy components are subjected to challenging conditions in high performance applications, consisting of complex loads and thermal gradients. To improve the performance and efficiency of such components, it is desirable to introduce different microstructures into subcomponent regions which cannot be achieved by the conventional melt-wrought processing route. Instead, a solid-state consolidation route using dissimilar titanium alloy powders is proposed. In this study commercially pure Ti (CP-Ti), Ti-6Al-4V (Ti-6-4), and Ti-5Al-5Mo-5V-3Cr (Ti-5553) have been diffusion bonded using field assisted sintering technology (FAST) for dwell times of 10, 20, and 60 min. The effectiveness of FAST for diffusion bonding (DB) of dissimilar alloy powders has led to the authors terming this hybrid process as "FAST-DB". Excellent bond integrity was produced with no cracking, unbonded regions or voids in the dissimilar bond combinations, at all dwell times. Furthermore, reliable control and prediction of the bond characteristics and degree of elemental diffusion was demonstrated through commercial thermodynamic software. Elemental diffusion was characterised across the bonds and the chemical diffusion bond width increased linearly with dwell time. Peak hardness values occurred directly on the interface for Ti-5553 and CP-Ti bonds, whilst slightly into the Ti-6-4 alloy for the Ti-5553 and Ti-6-4 bonds, which can be attributed to fine scale alpha at the interface. In Ti-6-4 with CP-Ti bonds, a smooth transition was observed. Mechanical testing demonstrated that the FAST-DB interface had excellent structural integrity, with necking and fracture occurring in the lower strength alloy. [ABSTRACT FROM AUTHOR]

The majority of NCEs are weakly basic drugs. Consequently, their solubility is highly pH-dependent, with higher solubility in the acidic stomach and poor solubility in the neutral intestinal environment. The gastric emptying of dissolved drug can lead to the intestinal precipitation of the drug. One option of reducing this process is to formulate the drug together with a precipitation inhibitor (PI). The aim of this study was to investigate the effects of different PIs on the intestinal concentrations of ketoconazole and five orally administered kinase inhibitors (i.e. pazopanib, gefitinib, lapatinib, vemurafenib, and a Merck KGaA research compound, MSC-A) with the aid of a predictive small-scale in vitro transfer model. This screening revealed that HPMCAS and Soluplus® were the most effective PIs. Whereas all other drugs precipitated within several minutes, gefitinib expressed highly variable amorphous precipitation which was confirmed by PXRD. During the transfer model experiments, this intermediate supersaturated state was stabilized using HPMCAS and Soluplus®. The PI screening protocol described herein allows to study the effect of PIs for solubility and potential bioavailability improvement of poorly soluble drugs to support formulation development already in early stages. [ABSTRACT FROM AUTHOR]

New nanocomposites of polyaniline nanofibers/titanium dioxide nanoparticles (PANINFs/TiO 2 NPs) from aniline hydrochloride salt, titanium dioxide nanoparticles (TiO 2 NPs) and FeCl 3• 6H 2 O as the oxidant were synthesized through a simple mechanochemical reaction in solid state and template-free technique. The PANINFs/TiO 2 NPs nanocomposite, polyaniline nanofibers (PANINFs) and TiO 2 NPs were characterized by field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), Fourier-transform infrared spectra, ultraviolet-visible spectra, cyclic voltammetry (CV) and electrical conductivity. TEM images clearly demonstrate that TiO 2 NPs are embedded in the PANINFs. Electrochemical calculations of band gap from CV curves indicated that the forbidden band gap of the PANINFs/TiO 2 NPs nanocomposite is 1.78 eV, realizing the complementary advantages of n and p semiconductors. Doctor blade method was used to prepare films for three kinds of hybrid solar cells in terms of different architectures such as ITO│TiO 2 NPs│PANINFs│Al , ITO│PANINFs/TiO 2 NPs│Al, and ITO│TiO 2 NPs│PANINFs/TiO 2 NPs│Al. Their I–V characteristics and power conversion efficiency (PCE) under 100 mWcm−2 irradiation and AM 1.5 global conditions were measured and discussed. The PCE of the three samples were 0.21, 0.38 and 0.91%, respectively. [ABSTRACT FROM AUTHOR]

Abstract We report, for the first time, an experimental study of interaction of metal-organic framework (MOF) with dimethyl sulfoxide (DMSO). Adsorption of DMSO on aluminum MOF Basolite A100 results in formation of the stoichiometric complex [A100] 2 [DMSO] 3. The solid-state synchronous fluorescence spectroscopy allows observation of the following major excitation/emission transitions in Basolite A100 and its adsorption complex [A100] 2 [DMSO] 3 which are not well-resolved in "conventional" fluorescence spectra: 1) narrow resonance of the isolated BDC linker, 2) excitation across optical bandgap, and 3) excimers. In the adsorption complex [A100] 2 [DMSO] 3 , the DMSO molecules interact with the μ 2 -OH group of Basolite A100 and with its BDC linker through the π-π system. We present, for the first time, the new variety of the solid-state synchronous fluorescence spectroscopy, which we denote as the solid-state enhanced-resolution synchronous fluorescence (excitation) spectroscopy. The accurate measurements of small changes in the optical bandgap of the adsorption complex [A100] 2 [DMSO] 3 and Basolite A100 are described by the solid-state enhanced-resolution synchronous fluorescence (excitation) spectroscopy. [ABSTRACT FROM AUTHOR]