Extraction of gamma iron oxide (γ-Fe2O3) nanoparticles from waste can: Structure, morphology and magnetic properties.

In this work, the transformation of waste iron cans to gamma iron oxide (γ-Fe2O3) nanoparticles following acid leaching precipitation method along with their structural, surface chemistry, and magnetic properties was studied. Highly magnetic iron-based nanomaterials, maghemite with high saturation magnetization have been synthesized through an acid leaching technique by carefully tuning of pH and calcination temperature. The phase composition and crystal structure, surface morphology, surface chemistry, and surface composition of the synthesized γ-Fe2O3 nanoparticles were explored by X-ray diffraction (XRD), Scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and Energy-dispersive X-ray spectroscopy (EDS). The XRD results confirm the cubic spinel structure having crystallite size 26.90-52.15 nm. The XPS study reveals the presence of Fe, O element and the binding energy of Fe (710.31 and 724.48 eV) confirms the formation of γ-Fe2O3 as well. By dynamic light scattering (DLS) method and zeta potential analyzer, the particle size distribution and stability of the systems were investigated. The magnetic behavior of the synthesized γ-Fe2O3 nanoparticles were studied using a vibrating sample magnetometer (VSM) which confirmed the ferrimagnetic particles with saturation magnetization of 54.94 emu/g. The resultant maghemite nanoparticles will be used in photocatalysts and humidity sensing. The net impact of the work stated here is based on the principle of converting waste into useful nanomaterials. Finally, it was concluded that our results can give insights into the design of the synthesis procedure from the precursor to the high-quality gamma iron oxide nanoparticles with high saturation magnetization for different potential applications which are inexpensive and very simple.

Comprehensive review of micro/nanostructured ZnSnO3: characteristics, synthesis, and diverse applications.

Generally, zinc stannate (ZnSnO3) is a fascinating ternary oxide compound, which has attracted significant attention in the field of materials science due to its unique properties such high sensitivity, large specific area, non-toxic nature, and good compatibility. Furthermore, in terms of both its structure and properties, it is the most appealing category of nanoparticles. The chemical stability of ZnSnO3 under normal conditions contributes to its applicability in various fields. To date, its potential as a luminescent and photovoltaic material and application in supercapacitors, batteries, solar cells, biosensors, gas sensors, and catalysts have been extensively studied. Additionally, the efficient energy storage capacity of ZnSnO3 makes it a promising candidate for the development of energy storage systems. This review focuses on the notable progress in the structural features of ZnSnO3 nanocomposites, including the synthetic processes employed for the fabrication of various ZnSnO3 nanocomposites, their intrinsic characteristics, and their present-day uses. Specifically, we highlight the recent progress in ZnSnO3-based nanomaterials, composites, and doped materials for their utilization in Li-ion batteries, photocatalysis, gas sensors, and energy storage and conversion devices. The further exploration and understanding of the properties of ZnSnO3 will undoubtedly lead to its broader implementation and contribute to the advancement of next-generation materials and devices.

Investigation of structural, morphological and magnetic properties of nanostructured strontium hexaferrite through co-precipitation technique: Impacts of annealing temperature and Fe/Sr ratio.

M-type strontium hexaferrite (SrM) were successfully synthesized from Sr2+ and Fe3+ precursor salt through co-precipitation technique. Different higher sintering temperatures (800-1000 °C) were used to get the desired SrM with variation of Fe3+/Sr2+ mole ratio as well. The characterization of SrM and its properties were investigated using modern instrumental techniques viz. X-ray diffraction (XRD), Fourier Transform Infrared Spectrometer, Scanning Electron Microscopy, Vibrating Sample Magnetometer, UV-Visible NIR Spectrometer, Impedance Analyzer and Thermal Conductivity Meter. The phase of the synthesized SrM were confirmed by comparing the XRD patterns with the standard ICDD data and Reitvelt Refinement for the SrM having Fe3+/Sr2+ ratio 10 and SrM with distinct annealing temperature were performed. The structural parameters, particle size (75 nm-318 nm) and shape of the as prepared samples were changed with calcination temperature as well as mole ratio. The saturation magnetization (73.77-24.27 emu/g), coercivity (3732.28-642.10 Oe) and remanant magnetization (39.15-8.86 emu/g) were varied with calcination temperature and composition. The dielectric properties, optical properties and thermophysical properties were measured for the SrM keeping Fe3+/Sr2+ ratio 10 calcined at 1000 °C. The synthesized SrM can be applied in magnetic recording media and as photocatalyst due to its low coercivity (2764.48 Oe), high saturation magnetization (73.77 emu/g) and low band gap energy (Eg-2.04 eV) respectively.

Combining Neural and Behavioral Measures Enhances Adaptive Training.

Adaptive training adjusts a training task with the goal of improving learning outcomes. Adaptive training has been shown to improve human performance in attention, working memory capacity, and motor control tasks. Additionally, correlations have been observed between neural EEG spectral features (4-13 Hz) and the performance of some cognitive tasks. This relationship suggests some EEG features may be useful in adaptive training regimens. Here, we anticipated that adding a neural measure into a behavioral-based adaptive training system would improve human performance on a subsequent transfer task. We designed, developed, and conducted a between-subjects study of 44 participants comparing three training regimens: Single Item Fixed Difficulty (SIFD), Behaviorally Adaptive Training (BAT), and Combined Adaptive Training (CAT) using both behavioral and EEG measures. Results showed a statistically significant transfer task performance advantage of the CAT-based system relative to SIFD and BAT systems of 6 and 9 percentage points, respectively. Our research shows a promising pathway for designing closed-loop BCI systems based on both users' behavioral performance and neural signals for augmenting human performance.

Natural Cellulosic Fiber Reinforced Concrete: Influence of Fiber Type and Loading Percentage on Mechanical and Water Absorption Performance.

The paper reports experimental research regarding the mechanical characteristics of concrete reinforced with natural cellulosic fibers like jute, sisal, sugarcane, and coconut. Each type of natural fiber, with an average of 30 mm length, was mixed with a concrete matrix in varying proportions of 0.5% to 3% mass. The tensile and compressive strength of the developed concrete samples with cellulosic fiber reinforcement gradually increased with the increasing proportion of natural cellulosic fibers up to 2%. A further increase in fiber loading fraction results in deterioration of the mechanical properties. By using jute and sisal fiber reinforcement, about 11.6% to 20.2% improvement in tensile and compressive strength, respectively, was observed compared to plain concrete, just by adding 2% of fibers in the concrete mix. Bending strength increased for the natural fiber-based concrete with up to 1.5% fiber loading. However, a decrease in bending strength was observed beyond 1.5% loading due to cracks at fiber-concrete interface. The impact performance showed gradual improvement with natural fiber loading of up to 2%. The water absorption capacity of natural cellulosic fiber reinforced concrete decreased substantially; however, it increased with the loading percent of fibers. The natural fiber reinforced concrete can be commercially used for interior or exterior pavements and flooring slabs as a sustainable construction material for the future.

Waste Fiber-Based Poly(hydroxamic acid) Ligand for Toxic Metals Removal from Industrial Wastewater.

Toxic metals in the industrial wastewaters have been liable for drastic pollution hence a powerful and economical treatment technology is needed for water purification. For this reason, some pure cellulosic materials were derived from waste fiber to obtain an economical adsorbent for wastewater treatment. Conversion of cellulose into grafting materials such as poly(methyl acrylate)-grafted cellulose was performed by free radical grafting process. Consequently, poly(hydroxamic acid) ligand was produced from the grafted cellulose. The intermediate products and poly(hydroxamic acid) ligand were analyzed by FT-IR, FE-SEM, TEM, EDX, and XPS spectroscopy. The adsorption capacity (qe) of some toxic metals ions by the polymer ligand was found to be excellent, e.g., copper capacity (qe) was 346.7 mg·g-1 at pH 6. On the other hand, several metal ions such as cobalt chromium and nickel also demonstrated noteworthy sorption capacity at pH 6. The adsorption mechanism obeyed the pseudo second-order rate kinetic model due to the satisfactory correlated experimental sorption values (qe). Langmuir model isotherm study showed the significant correlation coefficient with all metal ions (R2 > 0.99), indicating that the single or monolayer adsorption was the dominant mode on the surface of the adsorbent. This polymer ligand showed good properties on reusability. The result shows that the adsorbent may be recycled for 6 cycles without any dropping of starting sorption capabilities. This polymeric ligand showed outstanding toxic metals removal magnitude, up to 90-99% of toxic metal ions can be removed from industrial wastewater.

Synthesis of Silica-Supported Hydroxamic Ligand for Removal of Metals Ions from Water.

Mesoporous silica supported adsorbents have been used towards metal ion removal from water due to their thermally stability and good sorption capacity. Thus, mesoporous silica-based methyl acrylate monomer (Silica-APTES-DPNO) was converted into hydroxamic acid (SBHA) by using oximation reaction and all products are analyzed by by FT-IR. The SBHA showed satisfactory binding properties with copper, cobalt, nickel and lead are 242, 206, 195 and 516 mg g-1, respectively, with the batch adsorption system was set to pH 6. The kinetics of metal ions binding obeyed the pseudo-1st-order process up to 60 min. In this study also consider the Langmuir and Freundlich isotherm to find out the sorption behavior. The isotherm study demonstrated the well fit with Freundlich isotherm (R² > 0.99). Thus, adsorption take place as a multilayer system, therefore, SBHA material is useful for the metal ions removal from water.

Polymer Ligands Derived from Jute Fiber for Heavy Metal Removal from Electroplating Wastewater.

Industrial operations, domestic and agricultural activities worldwide have had major problems with various contaminants caused by environmental pollution. Heavy metal pollution in wastewater also a prominent issue; therefore, a well built and economical treatment technology is demanded for pollution-free wastewater. The present work emphasized pure cellulose extracted from jute fiber and further modification was performed by a free radical grafting reaction, which resulted in poly(methyl acrylate) (PMA)-grafted cellulose and poly(acrylonitrile)-grafted cellulose. Subsequently, poly(hydroxamic acid) and poly(amidoxime) ligands were prepared from the PMA-grafted cellulose and PAN-grafted cellulose, respectively. An adsorption study was performed using the desired ligands with heavy metals such as copper, cobalt, chromium and nickel ions. The binding capacity (qe) with copper ions for poly(hydroxamic acid) is 352 mg g-1 whereas qe for poly(amidoxime) ligand it was exhibited as 310 mg g-1. Other metal ions (chromium, cobalt and nickel) show significance binding properties at pH 6. The Langmuir and Freundlich isotherm study was also performed. The Freundlich isotherm model showed good correlation coefficients for all metal ions, indicating that multiple-layers adsorption was occurred by the polymer ligands. The reusability was evaluated and the adsorbents can be reused for 7 cycles without significant loss of removal performance. Both ligands showed outstanding metals removal capacity from the industrial wastewater as such 98% of copper can be removed from electroplating wastewater and other metals (cobalt, chromium, nickel and lead) can also be removed up to 90%.

Poly(amidoxime) ligand derived from waste palm fiber for the removal of heavy metals from electroplating wastewater.

A waste material known as palm oil empty fruit bunch (EFB) is used as a source of cellulose for the development of polymeric materials for the removal of metal ions from industrial wastewater. A poly(acrylonitrile)-grafted palm cellulose copolymer was synthesized by a conventional free radical initiating process followed by synthesis of a poly(amidoxime) ligand by oximation reaction. The resulting products were characterized by FT-IR, FE-SEM, EDX, TGA, DSC, and XPS. The poly(amidoxime) ligand was used to coordinate with and extract a series of transition metal ions from water samples. The binding capacity (qe) of the ligand with the metal ions such as copper, iron, cobalt, nickel, and lead were 260, 210, 168, 172, and 272 mg g-1, respectively at pH 6. The adsorption process followed the pseudo-first-order kinetic model (R2 > 0.99) and as well as the Freundlich isotherm model (R2 > 0.99) indicating the occurrence of a multi-layer adsorption process in the amidoxime ligand adsorbent. Results from reusability studies show that the ligand can be recycled for at least 10 cycles without any significant losses to its initial adsorption capacity. The synthesized polymeric ligand was shown to absorb heavy metals from electroplating wastewater with up to 95% efficiency.

Ion-Imprinted Polymer for Selective Separation of Cerium(III) Ions from Rare Earth Mixture.

Ion-imprinting polymers (IIPs) materials draw the great recognition because of the powerful selectivity to the desired metal ions. Therefore, the ion-imprinting polymer (Ce-IIP) was prepared by using cerium metal with amidoxime ligand as the complexing agent, in addition ethylene glycol dimethacrylate (EGDMA) and 2,2-azobisisobutyronitrile (AIBN) are crosslinking agent and free radical initiator, respectively. Aqueous HCl was applied to leach the cerium ions from the imprinted polymer for the creation of cavities of template, which is utilized for further cerium ions adsorption with high selectivity. The Ce-IIP was characterized by using ICP-MS, FE-SEM and also solid state analysis by UV-vis NIR spectroscopy. FT-IR study confirmed the complexation of the Ce-IIP was successful. The optimum pH was found to be 6 and the highest adsorption capacity was estimated about 145 mg g-1. Thus, the prepared Ce-IIP gave very good selectivity to cerium ions in the presence of lanthanide ions and also Ce-IIP can be reused 10 times without a substantial loss in adsorption capacity.

Cellulose Supported Pd(II) Complex Catalyzed Carbon-Carbon Bonds Formation.

Corn-cobs are an agro-industrial waste and composed of cellulose mostly. In this study cellulose was isolated from the waste corn-cobs and modified to polymeric hydroxamic acid palladium complex 1 and characterized by using a variety of spectroscopic methods such as field emission scanning electron microscopy (FE-SEM), energy-dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), X-ray powder diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and inductively coupled plasma atomic emission spectroscopy (ICP-AES). The complex 1 exhibited high catalytic activity towards Suzuki and Heck coupling reactions of activated and deactivated aryl halides to give the respective coupling products with high yield. Moreover, the complex 1 was recovered and recycled five times with no considerable loss of catalytic overall performance.

Tapioca Cellulose Based Copper Nanoparticles for Chemoselective N-Alkylation.

Biomaterials as a support for catalysts are of prime importance. Tapioca root which is an abundant biopolymer source was used to synthesize cellulose supported bio-heterogeneous poly(hydroxamic acid) copper nanoparticles (CuN@PHA) and was characterized by Fourier transform infrared spectroscopy (FTIR), ultraviolet­visible spectroscopy (UV-Vis), field emission scanning electron microscopy (FESEM), X-ray photoelectron spectroscopy (XPS), inductively coupled plasma atomic emission spectroscopy (ICP-AES), transmission electron microscopy (TEM) analyses. The tapioca cellulose supported CuN@PHA (50 mol ppm) effectively catalyzed N-alkylation reaction of aliphatic amines with α,ß-unsaturated compounds to give the corresponding alkylated products. High yields up to 95% were achieved for the converted products. The reusability of the cellulose supported nanoparticles was found to be excellent with no significant reduction of its catalytic activity over several cycles. The catalyst showed high catalytic activity having turnover number (TON) 18000 and turnover frequency (TOF) 2250 h⁻¹.

Bio-waste corn-cob cellulose supported poly(hydroxamic acid) copper complex for Huisgen reaction: Waste to wealth approach.

Corn-cob cellulose supported poly(hydroxamic acid) Cu(II) complex was prepared by the surface modification of waste corn-cob cellulose through graft copolymerization and subsequent hydroximation. The complex was characterized by IR, UV, FESEM, TEM, XPS, EDX and ICP-AES analyses. The complex has been found to be an efficient catalyst for 1,3-dipolar Huisgen cycloaddition (CuAAC) of aryl/alkyl azides with a variety of alkynes as well as one-pot three-components reaction in the presence of sodium ascorbate to give the corresponding cycloaddition products in up to 96% yield and high turn over number (TON 18,600) and turn over frequency (TOF 930h-1) were achieved. The complex was easy to recover from the reaction mixture and reused six times without significant loss of its catalytic activity.

Synthesis of new liquid crystals embedded gold nanoparticles for photoswitching properties.

A new series of liquid crystals decorated gold nanoparticles is synthesized whose molecular architecture has azobenzenes moieties as the peripheral units connected to gold nanoparticles (Au NPs) via alkyl groups. The morphology and mesomorphic properties were investigated by field emission scanning electron microscope, high-resolution transmission electron microscopy, differential scanning calorimetry and polarizing optical microscopy. The thiolated ligand molecules (3a-c) showed enantiotropic smectic A phase, whereas gold nanoparticles (5a-c) exhibit nematic and smectic A phase with monotropic nature. HR-TEM measurement showed that the functionalized Au NPs are of the average size of 2nm and they are well dispersed without any aggregation. The trans-form of azo compounds showed a strong band in the UV region at ∼378nm for the π-π(∗) transition, and a weak band in the visible region at ∼472nm due to the n-π(∗) transition. These molecules exhibit attractive photoisomerization behaviour in which trans-cis transition takes about 15s whereas the cis-trans transition requires about 45min for compound 5c. The extent of reversible isomerization did not decay after 10 cycles, which proved that the photo-responsive properties of 5c were stable and repeatable. Therefore, these materials may be suitably exploited in the field of molecular switches and the optical storage devices.

Crystal structure of 3-{5-[3-(4-fluoro-phen-yl)-1-isopropyl-1H-indol-2-yl]-1H-pyrazol-1-yl}indolin-2-one ethanol monosolvate.

The title indolin-2-one compound, C28H23FN4O·C2H6O, crystallizes as a 1:1 ethanol solvate. The ethanol mol-ecule is disordered over two positions with refined site occupancies of 0.560 (14) and 0.440 (14). The pyrazole ring makes dihedral angles of 84.16 (10) and 85.33 (9)° with the indolin-2-one and indole rings, respectively, whereas the dihedral angle between indolin-2-one and indole rings is 57.30 (7)°. In the crystal, the components are linked by N-H⋯O and O-H⋯O hydrogen bonds, forming an inversion mol-ecule-solvate 2:2 dimer with R 4 (4)(12) ring motifs. The crystal structure is consolidated by π-π inter-action between pairs of inversion-related indolin-2-one rings [inter-planar spacing = 3.599 (2) Å].

Crystal structure of 4-({(1E,2E)-3-[3-(4-fluoro-phen-yl)-1-isopropyl-1H-indol-2-yl]allyl-idene}amino)-5-methyl-1H-1,2,4-triazole-5(4H)-thione.

The title compound, C23H22FN5S, exists in a trans conformation with respect to the methene C=C and the acyclic N=C bonds. The 1,2,4-triazole-5(4H)-thione ring makes dihedral angles of 88.66 (9) and 84.51 (10)°, respectively, with the indole and benzene rings. In the crystal, mol-ecules are linked by pairs of N-H⋯S hydrogen bonds, forming inversion dimers with an R 2 (2)(8) ring motif. The dimers are linked via C-H⋯π inter-actions, forming chains along [1-10]. The chains are linked via π-π inter-actions involving inversion-related triazole rings [centroid-centroid distance = 3.4340 (13) Å], forming layers parallel to the ab plane.

Crystal structure of 4-({(1E,2E)-3-[3-(4-fluoro-phen-yl)-1-isopropyl-1H-indol-2-yl]allyl-idene}amino)-1H-1,2,4-triazole-5(4H)-thione.

The asymmetric unit of the titled compound, C22H20FN5S, comprises two independent mol-ecules (A and B), both of which have a trans conformation with respect to the methene C=C [1.342 (2) and 1.335 (2) Å] and the acyclic N=C [1.283 (2) and 1.281 (2) Å] bonds. In mol-ecule A, the triazole ring makes dihedral angles of 55.01 (12) and 18.17 (9)° with the benzene and indole rings, respectively. The corresponding dihedral angles for mol-ecule B are 54.54 (11) and 14.60 (10)°, respectively. In the crystal, mol-ecules are consolidated into -A-B-A-B- chains along [010] via N-H⋯N hydrogen bonds. The chains are further linked into layers parallel to the ac plane via π-π inter-actions involving inversion-related triazole rings [centroid-centroid distances = 3.3436 (11)-3.4792 (13) Å].

6-(Hex-5-en-yloxy)naphthalene-2-carb-oxy-lic acid.

The asymmetric unit of the title compound, C17H18O3, comprises three independent mol-ecules with similar geometries. In each mol-ecule, the carbonyl group is twisted away from the napthalene ring system, making dihedral angles of 1.0 (2), 1.05 (19)° and 1.5 (2)°. The butene group in all three mol-ecules are disordered over two sets of sites, with a refined occupancy ratio of 0.664 (6):0.336 (6). In the crystal, mol-ecules are oriented with respect to their carbonyl groups, forming head-to-head dimers via O-H⋯O hydrogen bonds. Adjacent dimers are further inter-connected by C-H⋯O hydrogen bonds into chains along the a-axis direction. The crystal structure is further stabilized by weak C-H⋯π inter-actions.

6-Cyanona-phthalen-2-yl 4-hexyl-benzo-ate.

In the title compound, C24H23NO2, a whole mol-ecule is disordered over two sets of sites with occupancies in a ratio of 0.692 (6):0.308 (6). In the major disorder component, the naphthalene ring system forms a dihedral angle of 68.6 (5)° with the benzene ring. The corresponding angle in the minor component is 81.6 (10)°. In the crystal, mol-ecules are linked into chains propagating along the b-axis direction via weak C-H⋯O hydrogen bonds. The crystal packing is further consolidated by weak C-H⋯π inter-actions.

Crystal structure of (E)-4-{2-[4-(all-yloxy)phen-yl]diazen-yl}benzoic acid.

The title compound, C16H14N2O3, has an E conformation about the azo-benzene [-N=N- = 1.2481 (16) Å] linkage. The benzene rings are almost coplanar [dihedral angle = 1.36 (7)°]. The O atoms of the carb-oxy-lic acid group are disordered over two sets of sites and were refined with an occupancy ratio of 0.5:0.5. The two disordered components of the carb-oxy-lic acid group make dihedral angles of 1.5 (14) and 3.8 (12)° with the benzene ring to which they are attached. In the crystal, mol-ecules are linked via pairs of O-H⋯O hydrogen bonds, forming inversion dimers. The dimers are connected via C-H⋯O hydrogen bonds, forming ribbons lying parallel to [120]. These ribbons are linked via C-H⋯π inter-actions, forming slabs parallel to (001).