Powder Diffraction Research Articles

Effects of Ni Loadings on the Structure and Morphology of Carbon Nanotubes Using Nickel Doped Iron Oxide Catalysts

AbstractIron oxide and their different doped iron oxide catalyst have been used for decades and are considered as efficient catalysts in several synthesis schemes including synthesis of carbon nanotubes. The iron oxide of the catalyst is abundant in nature, high catalytic activity at low over potentials, stability in basic media and low cost, making it environmentally and economically attractive. Nickel doped iron oxide catalyst have not been reported in the literature. Doping of nickel over iron oxide catalyst, different percentage 1 %, 5 %, 10 % and 20 % were done by impregnation method. The samples were characterized by X‐Ray powder Diffraction (XRD), Fourier‐Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscope (SEM), Energy Dispersive X‐ray (EDX) and Thermo Gravimetric Analysis (TGA). Nickel doped iron oxide was used as catalyst for the synthesis of carbon nanotubes (CNTs) and doping changed the morphology of carbon nanotube (CNTs). FTIR results confirmed the doping and presence of different functional groups. Chemical vapor deposition (CVD) was carried out for the synthesis of multiwall carbon nanotubes (MWCNTs) on nickel doped iron oxide catalyst for different percentage (1 %, 5 %, 10 % and 20 %) separately. CVD assembly was carried in tube furnace and the reaction was checked at two different temperature i.e 700 °C and 750 °C and using methane and compressed natural gas (CNG) as precursors. The catalyst was activated in the furnace at 800 °C for an hour. Methane and argon were used in proportion 2 : 1 inside the furnace. SEM showed formation of CNTs at 750 °C with CNG precursor. Formation of CNTs increased with increasing doping with this CNTs was confirmed by SEM.

Synthesis and Characterization of Acacia-Stabilized Doxorubicin-Loaded Gold Nanoparticles for Breast Cancer Therapy.

The targeted delivery of drugs is vital in breast cancer treatment due to its ability to produce long-lasting therapeutic effects with minimal side effects. This study reports the successful development of doxorubicin hydrochloride (DOX)-loaded colloidal gold nanoparticles stabilized with acacia gum (AG). Optimization studies varied AG concentrations (0.25% to 3% w/v) to determine optimal conditions for nanoparticle synthesis. The resulting acacia stabilized gold nanoparticles (AGNPs) were characterized using various techniques including high-resolution transmission electron microscopy (HR-TEM), powder X-ray diffraction (PXRD), differential scanning calorimetry (DSC), ultraviolet-visible spectroscopy, Fourier-transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM), and selected area electron diffraction (SAED). In vitro drug release studies demonstrated a higher release rate of DOX in sodium acetate buffer (pH 5.0) compared to phosphate buffer saline (pH 7.4), suggesting an enhanced therapeutic efficacy in acidic tumor environments. Cytotoxicity of DOX-AGNPs and free DOX was assessed in human breast cancer cells (MDA-MB-231). The DOX-AGNPs exhibited significantly greater cytotoxicity, indicating enhanced efficacy in targeting cancer cells. This enhancement suggests that adsorbing DOX on the surface of gold nanoparticles can improve drug delivery and effectiveness, potentially reducing side effects compared to pure DOX and traditional delivery methods. Stability tests conducted over six months at 25±1°C showed significant changes in particle size and PDI, suggesting limited stability under these conditions. Overall, the acacia-stabilized gold nanoparticles synthesized in this study exhibit promising characteristics for drug delivery applications, particularly in cancer therapy, with effective drug loading, controlled release, and favorable physicochemical properties.

Crystal structure, Hirshfeld surface analysis, and DFT theoretical studies of an azobenzene derivative from powder X-ray diffraction

Crystal structure, Hirshfeld surface analysis, and DFT theoretical studies of an azobenzene derivative from powder X-ray diffraction

Pore Structures in Detritusphere of Soils Under Switchgrass and Restored Prairie Vegetation Community

ABSTRACTRoot detritusphere, that is, the soil in the vicinity of decomposing root residues, plays an important role in soil microbial activity and C sequestration. Pore structure (size distributions and connectivity of soil pores) in the detritusphere serves as a major driver for these processes and, in turn, is influenced by the physical characteristics of both soil and roots. This study compared pore structure characteristics in the root detritusphere of soils of contrasting texture and mineralogy subjected to > 6 years of contrasting vegetation: monoculture switchgrass and polyculture prairie systems. Soil samples were collected from five experimental sites in the US Midwest representing three soil types. Soil texture and mineralogy were measured using a hydrometer and x‐ray powder diffraction, respectively. The intact cores were scanned with x‐ray computed micro‐tomography to identify visible soil pores, biopores, and particulate organic matter (POM). We specifically focused on pore structure within the detritusphere around the POM of root origin. Results showed that the detritusphere of coarser textured soils, characterized by high sand and quartz contents, had lower porosity in the vicinity of POM compared with finer textured soils. POM vicinities in finer textured soils had high proportions of large (> 300 μm diameter) pores, and their pores were better connected than in the coarser soils. Lower porosity in the outer (> 1 mm) parts of the detritusphere of switchgrass than of prairie suggested soil compaction by roots, with the effect especially pronounced in the coarser soils. The results demonstrated that soil texture and mineralogy played a major, while vegetation played a more modest, role in defining the pore structure in the root detritusphere.

Growth, characterization and cognition of 2-cyanopyridinium perchlorate single crystals for nonlinear optical applications.

The fascinating electronic applications attracted researchers to explore the field of nonlinear optical (NLO) materials. The slow evaporation of solvent technique (SEST) was employed to grow the 2-cyanopyridinium perchlorate (2-CPPC) NLO single crystals. The cell parameters of the grown 2-CPPC crystal are confirmed by the single crystal X-ray diffraction (SCXRD) study. The powder X-ray diffraction studies confirm the crystallinity of 2-CPPC crystals, and the peaks were indexed. The computation for the geometry optimization, HOMO-LUMO energy gap, global reactivity parameters, natural bond orbital (NBO) analysis, polarizability, and hyperpolarizability of the 2-CPPC molecule was done using B3LYP (6-311G basis set) functional of DFT method. The experimental FTIR and UV-Vis results of the 2-CPPC compound were compared with the simulated results. The second harmonic generation (SHG) study for the 2-CPPC crystal was employed using Kurtz-Perry powder technique. Single beam Z-scan technique using He-Ne laser is used to study the third-order NLO properties.

Establishing Composition of Solid Solution Based on Single Crystal and Powder X-ray Measurement: The Case of Halogenated Bismuth(III) Complexes with Acetophenone-4-methyl-3-thiosemicarbazone

New bismuth (III) complexes with acetophenone-4-methyl-3-thiosemicarbazone (L) and halogens (Cl and Br) in both bridging and terminal positions have been synthesized and structurally characterized using single-crystal X-ray diffraction. The pure complexes (Cl or Br) were found to be highly isostructural, which motivated our attempts to create solid solutions of these complexes. A series of such compounds was prepared using various procedures and stoichiometries. A method for determining the mutual concentrations of different halogens, based on the positions of selected peaks in powder diffraction patterns, was tested and compared with other methods.

Synthesis and Luminescent Properties of TiO<sub>2</sub> Materials Single and Triple Doped with Rare Earth Ions (Sm<sup>3+</sup> , Tb <sup>3+</sup> and Eu<sup> 3+</sup>)

Four types of titanium dioxide (TiO2) materials doped with a single kind of rare earth ions Ln3+ (Eu3+, Tb3+, or Sm3+) and three rare earth ions (Eu3+, Tb3+, and Sm3+) were synthesized by the sol-gel method. The compositions, structures, and photophysical properties of these compounds were tested. The structure of the rare earth ion-doped TiO2 samples was characterized by X-ray powder diffraction (XRD) and Fourier-transform infrared spectroscopy (FT-IR). Optical absorption and fluorescence information was obtained using UV-Vis spectroscopy and fluorescence spectroscopy. The surface morphology of rare earth ion-doped TiO2 materials was observed using scanning electron microscopy (SEM). To further explore the photoluminescent properties of rare earth-doped TiO2 materials for practical applications, small-scale LED light-emitting devices were fabricated.

Impact of Ball Milling on the Microstructure of Polyethylene Terephthalate.

Polyethylene terephthalate (PET) is a semi-crystalline polymer that finds broad use. Consequently, it contributes to the accumulation of plastics in the environment, warranting PET recycling technologies. Ball milling is a commonly used technique for the micronization of plastics before transformation. It has also recently been reported as an efficient mixing strategy for the enzymatic hydrolysis of plastics in moist-solid mixtures. However, the effect of milling on the microstructure of PET has not been systematically investigated. Thus, the primary objective of this study is to characterize the changes to the PET microstructure caused by various ball milling conditions. PET of different forms was examined, including pre- and post-consumer PET, as well as textiles. The material was treated to a range of milling frequencies and duration, before analysis of particle size, crystallinity by differential scanning calorimetry and powder X-ray diffraction, and morphology by scanning electron microscopy. Interestingly, our results suggest the convergence of crystallinity to ~30% within 15 minutes of milling at 30 Hz. These results are consistent with an equilibrium between amorphous and crystalline regions of the polymer being established during ball milling. The combined data constitutes a reference guide for PET milling and recycling research.

Photocatalytic Degradation of Mancozeb Pesticide Residue using Nanoceria Doped Zinc Oxide Nanoparticles under Natural Solar Irradiation

Introduction: Excessive applications of agrochemicals to meet the high food demand from ever-increasing populations are becoming a major issue for both health practitioners and environmental managers. Chemicals such as ethylene bis-dithiocarbamate pesticide mancozeb (MCZ) are known to have deleterious effects on the ecosystem. AIM: This study, aimed at assessing the suitability of cerium-doped zinc oxide (Ce-ZnO) for efficient degradation of MCZ fungicide. Method: The photocatalysts were synthesized using the coprecipitation method with zinc nitrate hexahydrate, cerium nitrate hexahydrate, and sodium hydroxide. The synthesized nanocomposites were further characterized by Powder X-ray Diffraction (PXRD), Fourier Transform Infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), and Energy Dispersive X-ray Spectroscopy (EDAX). The average crystallite size of the as-synthesized particles was found to be 31.42 nm, with very sharp PXRD peaks revealing the pure crystal nature of the particles. The photocatalytic degradation activity was evaluated following a series of experiments under natural environmental conditions. The optimal conditions for the degradation of MCZ fungicide using Ce-ZnO were found to be 10 ppm initial concentration of MCZ, 20 mg dose of the Ce- ZnO photocatalyst, 180 minutes irradiation time, and 10-11 atmospheric UV index. Result: At the optimum conditions, the degradation efficiency was found to be about 90% after 180 minutes. The reported photocatalytic degradation of MCZ using Ce-ZnO fits a pseudo-firstorder kinetic model with an R2 value of 0. 9677. Similarly, the reusability of the as-synthesized photocatalyst was evaluated and found to be active for five rounds with little change in the activity. Conclusion: Thus, the degradation method in the current study can be suitable for the degradation and removal of MCZ in agricultural runoff in the field.

Copper-Based Metal–Organic Framework: Synthesis, Characterization and Evaluation for the Hydrogenation of Furfural to Furfuryl Alcohol

AbstractA novel Cu-MOF was synthesized at room temperature from commercially available and inexpensive reagents. The pre-catalyst was characterized using X-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, inductively coupled plasma-optical emission spectroscopy, Fourier transform-infrared spectroscopy, powder X-ray diffraction, Brunauer-Emmet-Teller (BET) and scanning electron microscopy-energy dispersive X-ray spectroscopy. The Cu-MOF was characterized as microporous material with BET surface area and pore volume of 7.47 m2/g and 0.27 cm3/g, respectively, and is stable in most solvents. The MOF was evaluated as a heterogeneous catalyst for the hydrogenation of furfural to furfuryl alcohol (FA). Cu-MOF exhibited a high conversion of FF (76%) with selectivity towards FA (100%) at 140 °C, 50 bar for 24 h. The MOF was reused four consecutive times with a loss in catalytic performance. The decrease in catalytic activity could be attributed to the formation of inactive Cu(0) as revealed by HR-TEM and XPS studies. The HR-TEM of spent Cu-MOF showed a uniform particle size diameter of 3.5 nm. This work is significant in providing new strategies for the design and fabrication of highly selective MOF catalysts for the FF upgrading.

Unveiling the NLO Potential of New Zn (II) Complex of 6‐Methylpyridine‐2‐Carboxaldehyde: Experimental/DFT Study on Spectral, Static, and Frequency‐Dependent Linear/Nonlinear Optical Parameters

ABSTRACTOngoing exploration focuses on synthesizing and characterizing coordination compounds to improve the design of nonlinear optical (NLO)‐based materials. In this regard, to examine spectral and static/frequency–dependent linear/NLO parameters, the new Zn (II) complex {[Zn(6‐MePyAld)2(Cl)]; 6‐MePyAld: 6‐methylpyridine‐2‐carboxaldehyde} was synthesized and characterized by using 1H and 13C NMR, mass (LC‐HRMS), powder XRD, and FTIR spectra. The electronic features of synthesized complex were investigated by considering the TD‐CAM‐B3LYP/ and TD‐M06L/6‐311G(d,p)//LanL2DZ levels of time‐dependent density functional theory (TD‐DFT). Moreover, the theoretical linear optical (LO), second‐, and third‐order NLO susceptibility tensors/polarization (χ(1)/P(1), χ(2)/P(2), χ(3)/P(3)) parameters for the Zn (II) complex were computed using the DFT/M06L and DFT/CAM‐B3LYP levels. The external electric field (E), polarization (P), and electric displacement (D) values of the Zn (II) complex were also calculated using the same DFT levels. To investigate microscopic LO (isotropic polarizability <α(0;0)>/<α(−ω;ω)>, and anisotropic polarizability (∆α (0;0)/∆α (−ω;ω)) and second‐/third‐order NLO (<β(0;0,0)>/<β(−ω;ω,0), <β(−2ω;ω,ω)>/<γ(0;0,0,0)>/<γ(−ω;ω,0,0)> and <γ(−2ω;ω,ω,0)>) parameters for the Zn (II) complex, the DFT/M06L and DFT/CAM‐B3LYP levels in the gas phase were used. The ∆α (0;0), ∆α (−ω;ω), <β(0;0,0)>, <β(−ω;ω,0)>, and <β(−2ω;ω,ω)> for Zn (II) complex were computed at 17.288 × 10−24, 21.782 × 10−24, 14.692 × 10−30, 466.80 × 10−30, and 210.79 × 10−30 esu, respectively, by using the DFT/CAM‐B3LYP level. Moreover, the <γ(0;0,0,0)>/<γ(−ω;ω,0,0)> and <γ(−2ω;ω,ω,0)> in the gas phase computed at the DFT/CAM‐B3LYP level for Zn (II) complex were obtained at 129.74 × 10−36, 3997.6 × 10−36, and −886.60 × 10−36 esu, in turn. According to the CAM‐B3LYP level, the <γ(0;0,0,0)> value is 8.65 and 18.53 times higher than the values of para‐nitroaniline (pNA) and urea, respectively. The obtained static/dynamic β and γ values of Zn (II) complex are greater than those of urea and pNA. Zn (II) complex exhibited remarkably microscopic second‐order and particularly third‐order NLO features. It is predicted that our study will shed light on NLO materials that might be used in telecommunication and optoelectronics.

Green Synthesis of New Derivatives of Iminothiazole Using Cefixime and Removing Organic Pollutants from Aqueous Environment by Employing Cu@KF/Clinoptilolite NPs.

In this research, multicomponent reactions of cefixime, isothiocyanates, and alkyl bromides were carried out for the synthesis of new iminothiazole derivatives with high yields in water as the solvent at room temperature in the presence of catalytic amounts of Cu@KF/CP NPs as catalysts. Also, the ability of Cu@KF/Clinoptilolite nanoparticles (NPs) to adsorb and remove 4-NP and cefixime from water was investigated. The Cu@KF/Clinoptilolite nanoparticles were synthesized by employing a water extract of Petasites hybridus rhizomes. For this experiment, all of the components obtained from Fluka and Merck were subjected to further purification. The antibiotic used in this investigation, cefixime, was obtained from a pharmaceutical facility situated in Sari, Mazandaran, Iran. The antibiotic factory is located in Sari City, Iran. All solutions were prepared using distilled water. The shape of Cu@KF/CP nanoparticles was analyzed using images obtained from a Holland Philips XL30 scanning electron microscope. An analysis was performed on the crystalline structure of Cu@KF/CP nanoparticles (NPs), and a room temperature X-ray diffraction (XRD) examination was carried out utilizing a Holland Philips Xpert X-ray powder diffractometer. The X-ray diffraction (XRD) examination was conducted using CuK radiation, which has a wavelength of 0.15406 nm. The analysis covered a 2ε angle range from 20 to 80°. The nanostructures that were produced were chemically analyzed using X-ray energy dispersive spectroscopy (EDS) with an S3700N equipment. The morphology and dimensions of Cu@KF/CP nanoparticles were characterized using a Philips EM208 transmission electron microscope operated at an acceleration voltage of 90 kV. The primary objective of this study was to develop a sustainable approach for producing new iminothiazole derivatives 4. This was achieved using a highly efficient three-component reaction combining cefixime 1, isothiocyanates 2, and alkyl bromides 3. The reaction was carried out in water at ambient temperature, using Cu@KF/CP NPs as a highly effective catalyst, leading to excellent yields. Moreover, the study findings showed that the synthesized compounds demonstrated a significant antioxidant activity compared to conventional antioxidants. The antibacterial efficacy of the synthesized compounds was evaluated against both Gram-positive and Gram-negative bacteria. Furthermore, Cu@KF/CP nanoparticles were utilized to adsorb CFX and 4-NP from water-based solutions. This study showcases the effective synthesis of innovative iminothiazole derivatives through the use of multicomponent reactions, involving the combination of cefixime, isothiocyanates, and alkyl bromides. The reactions were conducted in a water-based solvent. The reactions were carried out at room temperature, utilizing Cu@KF/CP NPs as catalysts. The Cu@KF/CP nanoparticles, a newly developed heterogeneous nanocatalyst, were synthesized and evaluated utilizing X-ray diffraction (XRD), fieldemission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), and transmission electron microscopy (TEM) research techniques. Cu@KF/CP nanoparticles are utilized to adsorb CFX and 4-NP from water-based solutions. The objects were manufactured using a straightforward and uncomplicated approach. The BET surface area of Cu@KF/CP NPs was measured to be 201.8 m2/g. The experimental equilibrium data was evaluated by applying the isotherms of the Langmuir, Freundlich, Dubinin-Radushkevich, and Redlich-Peterson models. Additionally, we examined the catalytic efficiency of Cu@KF/CP nanoparticles (NPs) in reducing various colors in water.

Organotin(IV) complexes of tridentate (ONO) hydrazone ligands: synthesis, spectral characterization, antituberculosis, antimicrobial, anti-inflammatory, molecular docking and cytotoxicity studies.

Infectious diseases have a significant impact in the historical trajectory of humanity, exerting profound influence on societies, driving advancements in medical science, and significantly impacting individuals on a worldwide scale. Consequently, this research endeavours to identify potent agents combatting tuberculosis, inflammation, and microbial deformities. The investigation focuses on hydrazones (1,2) endowed eight organotin(IV) complexes, where hydrazones were derived from 2-acetyl-1H-indene-1,3(2H)-dione and 2-phenoxypropanehydrazide/2-(2,4-dichlorophenoxy)propanehydrazide. All compounds underwent thorough characterization utilizing a variety of spectral and analytical techniques including, multinuclear NMR, FT-IR, HRMS, UV-Vis, SEM-EDAX, TGA, XRD, molar conductance measurements, establishing the pentacoordinated environment around tin(IV) ion with tridentate (ONO) mode of chelation of hydrazones. Powder XRD revealed the ligand's crystalline and complexes' semi-crystalline nature, while thermal analysis indicated two-step decomposition leaving tin oxide residue. In vitro evaluations utilize microplate alamar blue assay for assessing anti-tuberculosis activity, serial dilution technique for antimicrobial efficacy, and bovine serum albumin method for evaluating anti-inflammatory properties. The complexes exhibited higher biological activities than their respective ligands and the activity of the complexes follow the order: Ph2SnL1-2 > Bu2SnL1-2 > Et2SnL1-2 > Me2SnL1-2. Among them, phenyl complex (10) [Ph2SnL2] displays superior efficacy against TB dysfunction (MIC: 0.0180 ± 0.009μmol/mL) and also demonstrates exceptional potency in combating inflammation (IC50: 7.27 ± 0.04μM), and microbial (MIC: 0.0045μmol/mL) infections, comparable to standard drugs. Additionally, cytotoxicity testing against vero cell line revealed decreased toxicity at lower concentrations, and attenuated by chelation. Phenyl complex (10) [Ph2SnL2] shows promising cytotoxicity at 3.12µg/mL (19.29 ± 0.09%). Further, The diphenyltin(IV) complex (10), identified as the most effective against TB, shows stronger binding to key 3PTY protein residues (-42.2kJ/mol) compared to ligand (2) (-33.4kJ/mol), correlating with its superior anti-tuberculosis potency in biological assays. This comprehensive approach aims to actively contribute to ongoing initiatives addressing infectious diseases, thereby advancing global health and overall well-being.

The Effect of Sodium Hexametaphosphate on the Dispersion and Polishing Performance of Lanthanum–Cerium-Based Slurry

A lanthanum–cerium-based abrasive composed of CeO2, LaOF, and LaF3 was commercially obtained. The effect of sodium hexametaphosphate (SHMP) on powder dispersion behavior was systematically investigated using the combined techniques of liquid contact angle, turbidity, zeta potential (ZP), scanning electron microscopy (SEM), powder X-ray diffraction (XRD) combined with Rietveld refinements, X-ray photoelectron spectroscopy (XPS), and polishing tests. The results indicated that the addition of 0.5 wt.% SHMP dispersant to the 5 wt.% lanthanum–cerium-based slurry produced the most stable suspension with a high turbidity of 2715 NTU and a low wetting angle of 45°. The as-obtained slurry displayed good surface polishing quality for K9 glass, with low surface roughness (Ra) of 0.642 and 0.515 nm (in the range of 979 × 979 μm2) at pH = 6 and 11, respectively, which corresponds to the fact that it has local maximum absolute values of ZP at these two pH values. SEM images demonstrated that after appropriate grafting of SHMP, the particle aggregation was reduced and the slurry’s dispersion stability was improved. In addition, the dispersion mechanism was explained based on the principle of complexation reaction, which reveals that the dispersant SHMP can increase the interparticle steric hindrance and electrostatic repulsions. In an acidic environment, steric hindrance dominates, while electrostatic repulsion prevails under alkaline conditions. As expected, this polishing slurry may find potential applications in manufacturing optical devices and integrated circuits.

Design of a Nickel mixed-ligand coordination compound for the removal of pollutant dye, methyl orange, from water

We report the uptake of methyl orange (MO) dye from aqueous solution by a synthesized Ni(II) complex. Characterization of the complex was achieved by powder X-ray diffraction (PXRD) analysis, Fourier transform infrared (FTIR) spectroscopy, Brunauer–Emmett–Teller (BET) analysis, and Scanning Electron Microscopy (SEM). BET surface area values were observed to be 252.450 m2 g−1 before adsorption and 242.260 m2 g−1 after adsorption. SEM micrographs showed a change in the morphology of the compound after adsorption. Adsorption experiments carried out at different conditions of dye concentration, pH of dye solution, contact time, dosage and temperature showed that the adsorption data best fits the Freundlich Isotherm with an R2 value of 0.9532 and adsorption process followed the pseudo-second-order kinetics equation (R2 = 0.9898).

“Synthesis and characterization of TiO2 nanoparticles as brake fluid additives: Viscosity modulation and impact on rheological properties”

TiO2 nanoparticles were synthesized using the reduction precipitation method, verified by powder x-ray diffraction (PXRD) with an average crystallite size of 62 nm and an average particle size of 135 nm from SEM images. Rheological studies of brake fluid with nanoparticle additives revealed that while the fluid generally maintains consistent behavior, a 2 wt.% concentration showed non-Newtonian behavior at 120 °C. Viscosity increased slightly with nanoparticle addition and decreased with rising temperature, with the 0.5 wt.% sample demonstrating the most notable increase of 18.18% at 120 °C. At 30 °C, the 1 wt.% sample exhibited a 4.06% increase. The observed viscosity changes are attributed to higher internal shear stress and the need to manage dispersion solid elements. The Herschel-Bulkley model was effective in predicting sample behavior, and all samples conformed to Reynolds’ equation μ 0 = b e − aT . This research indicates that TiO2 nanoparticles can be effectively used as brake fluid additives, offering potential benefits for high-temperature applications in vehicles. Further optimization using mathematical models such as response surface methodology (RSM) is suggested for improved performance.

Aloebarbadensis - Assisted MgBiO/MgCuBiO/MgBaBiO nanocomposites as effective gamma shielding novel materials

For the first of its kind, MgO/Bi2O3 (1:1) (MBO), MgO/CuO/Bi2O3 (1:1:1) (MCBO) and MgO/BaO/Bi2O3 (1:1:1) (MBBO) binary/ternary nanocomposites (NCs) were synthesized by Aloe barbadensis (Aloe vera) mediated solution combustion method. The as-formed NCs are subjected to calcination for 3 h at 600oC.The Mg-based NCs acquired are subjected to various analytical characterization methodologies, including PXRD (Powder X-ray Diffraction), SEM (Scanning Electron Microscopy), EDS (Energy Dispersive X-ray Spectroscopy), FTIR (Fourier Transform Infrared Spectroscopy), and Ultraviolet–Visible Spectroscopy (UV–Vis). The Bragg reflections confirm the formation of monoclinic phase BaO, Bi2O3, cubic MgO and tetragonal CuO nanoparticles. The surface morphology of MBO, MCBO and MBBO NCs consists of irregular sized, leafy and burrow like structured agglomerated NPs with hollows and voids/pores. The Eg (direct energy band gap) determined from W-H (Wood and Tauc's) plot was found to be 3.09, 3.19 and 3.12 eV for MBO, MCBO and MBBO NCs respectively. The evaluation of gamma radiation shielding properties was conducted using a NaI (Tl) detector connected to a multi-channel analyzer. Shielding parameters of MBO, MCBO and MBBO, such as μ/ρ (mass attenuation coefficient), λ (mean free path), HVL (half-value layer), TVL (tenth-value layer) are measured. Among the as-synthesized Mg-based NCs, MBO exhibits better shielding properties compared to MCBO and MBBO. Thus, the procured Mg-based NCs are suitable for applications where weight reduction is critical, such as aerospace or portable radiation shielding systems.

Characterization and Crystal Structural Analysis of Novel Carvedilol Adipate and Succinate Ethanol-Solvated Salts

Two ethanol-solvated adipate and succinate salts of carvedilol (CVD), a Biopharmaceutics Classification System class 2 drug, were synthesized by crystallizing ethanol with adipic acid (ADP) and succinic acid (SUA). Proton transfer from ADP and SUA to CVD and the presence of ethanol in the two novel compounds were confirmed using powder X-ray diffraction, Fourier transform infrared spectroscopy, differential scanning calorimetry, thermogravimetric analysis, and single-crystal X-ray diffraction measurements. The two novel ethanol-solvated salts exhibited enhanced solubility and dissolution rates compared with pure carvedilol in phosphate buffer (pH 6.8). Additionally, the morphologies and attachment energies of the two novel compounds and pure CVD were calculated based on their single-crystal structures, revealing a correlation between attachment energy and dissolution rate.

Catalytic and Electrochemical Study of Cu-ZSM-5/MCM-41.

Hierarchically structured micro-mesoporous ZSM-5/MCM-41 composite materials incorporating copper ions were synthesized using pre-synthesized ZSM-5 and cetyltrimethylammonium bromide (CTAB) as a template for forming the MCM-41 structure. The composites were characterized through powder X-ray diffraction, N2 adsorption-desorption, diffuse reflectance spectroscopy (UV-vis DRS), Fourier transform infrared spectroscopy, thermogravimetric analysis, scanning electron microscopy, and energy dispersive X-ray spectroscopy. X-ray diffraction confirmed well-ordered ZSM-5 and MCM-41 structures, and UV-vis DRS showed successful copper ion incorporation. N2 adsorption-desorption revealed the presence of both microporous and mesoporous structures. To evaluate their catalytic performance, Cu-incorporated ZSM-5/MCM-41 composite catalysts were assessed through the oxidation reaction of ethylbenzene using tert-butyl hydroperoxide (TBHP) as the oxidizing agent. With a 9% (w/w) Cu-ZM-5 (5 wt % copper-incorporated ZSM-5/MCM-41) catalyst and an oxidant to ethylbenzene molar ratio of 2:1 at 40 °C in the absence of a solvent for 4 h, the process yielded acetophenone (93.2%) as the major product. Additionally, these Cu-incorporated composites were examined as electrode materials for electrochemical storage. Cyclic voltammetry and galvanostatic charge-discharge studies showed that Cu-ZM-5 exhibited pseudocapacitive behavior, with a capacitance of up to 366 F g-1 at a current density of 1 A g-1, surpassing ZSM-5 and ZSM-5/MCM-41. These results highlight Cu-ZM-5's potential as an effective electrode material for electrochemical storage applications like supercapacitors.

Lattice symmetry relaxation as a cause for anisotropic line broadening and peak shift in powder diffraction.

In powder diffraction, lattice symmetry relaxation causes a peak to split into several components which are not resolved if the degree of desymmetrization is small (pseudosymmetry). Here the equations which rule peak splitting are elaborated for the six minimal symmetry transitions, showing that the resulting split peaks are generally broader and asymmetric, and suffer an hkl-dependent displacement with respect to the high-symmetry parent peak. These results will be of help in Rietveld refinement of pseudosymmetric structures where an exact interpretation of peak deformation is required.