Crystallite Size Research Articles

Fabrication of bare and cobalt-doped ZnFe2O4 thin film as NH3 gas sensor with enhanced response through UV-light illumination

This work reports on the deposition of bare and cobalt-doped ZnFe2O4 thin films by chemical spray pyrolysis technique to study ammonia (NH3) gas sensing properties. Colorless and strongly smelling, ammonia (NH3) is readily soluble in water and yields ammonium (NH) ions. These gases mix in the air atmosphere cause climate change, and severely affect human health. Therefore, the detection of NH3 below the exposure limit can avoid the deterioration of human health and environment. Co-doping had a significant effect on surface roughness, surface morphology, crystallite size, and sensitivity at room temperature. Co0.5Zn0.5Fe2O4 film (ZFCO5) exhibited an outstanding response (S = 19) towards 10 ppm NH3 gas at room temperature. Compared to the bare film, the ZFCO5 sensor has an eleven-fold higher gas-detection response value for 10 ppm NH3. This is ascribed to the blended effects of small crystallite size, high surface roughness, oxygen vacancies, and angular shape morphology linked into tiny rods in the ZFCO5 film. The ZFCO5 sensor showed a significant speedup in response/recovery times (102 s/34 s) and good response (S = 25) to NH3 under the UV-light (365 nm) illumination at room temperature. The built-in ZFCO5 gas sensor shows promise for real-time NH3 below threshold level monitoring.

An investigation for optical, photocatalytic, photoluminescence and dielectric properties of Cd0.40Ni0.60ZnO2 annealed nanocomposites

We report here the optical, photoluminescence (PL), and dielectric properties of Cd0.40Ni0.60ZnO2 nanocomposites annealed between 200 and 600oC. An increase in annealing temperature (Tann) up to 600oC correlates with a gradual increase in the crystallite and particle sizes. The surface area, pore radius, and pore volume are increased as Tann increases from 200oC to 300oC, and then decreased, but still higher than of 200oC. Similar behaviors were obtained for the absorbance carrier density, photocatlytic efficiency, degradation rate, PL intensity, dielectric constant, dielectric loss, ac conductivity, F-factor, series resistance, and electronic polarizability. While the energy gap, binding energy, impedance of grains and their boundaries, and effective capacitance show an opposite behavior. The relaxation times at the peak of dielectric parameters are between 11.54 and 159.24ns and between 35.23 and 24273.73ns, respectively. The Cole-Cole plot shows a single semicircle at Tann < 400oC and two successive semicircles at Tann> 500oC. The energy of PL of visible emissions is independent on the chosen Tann. These findings indicated that the nanocomposite annealed at 300oC can be used for water purification, telecommunications, solar cells, supercapacitor, and white light-emitting diodes (LEDs).

Fabrication and characterization of methylammonium lead iodide-based perovskite solar cells under ambient conditions

&lt;p&gt;This study investigated the fabrication and characterization of CH&lt;sub&gt;3&lt;/sub&gt;NH&lt;sub&gt;3&lt;/sub&gt;PbI&lt;sub&gt;3&lt;/sub&gt; based perovskite solar cells (PSCs) using the one-step spin coating technique under ambient conditions, eliminating the need for expensive glovebox and thermal evaporation equipment. The perovskite layer was annealed at 65 °C for 30 seconds and 100 °C for 30 seconds, 1 and 2 minutes. The scanning electron microscope (SEM) images show a smooth and uniform surface coverage for the ETL and CH&lt;sub&gt;3&lt;/sub&gt;NH&lt;sub&gt;3&lt;/sub&gt;PbI&lt;sub&gt;3&lt;/sub&gt; layers. SEM results also show an average grain size of 397 nm for CH&lt;sub&gt;3&lt;/sub&gt;NH&lt;sub&gt;3&lt;/sub&gt;PbI&lt;sub&gt;3&lt;/sub&gt; and an average particle size of ~17 nm for TiO&lt;sub&gt;2&lt;/sub&gt; was confirmed by transmission electron microscopy (TEM). X-ray diffraction (XRD) results confirmed the formation of tetragonal perovskite (CH&lt;sub&gt;3&lt;/sub&gt;NH&lt;sub&gt;3&lt;/sub&gt;PbI&lt;sub&gt;3&lt;/sub&gt;) phase with high crystallinity with a crystallite size of 19.99 nm for the samples annealed for 30 seconds at 65 °C and 1 min at 100 °C. FTIR results also confirmed the presence of anatase TiO2 at wavenumber 438 cm&lt;sup&gt;-1&lt;/sup&gt; and the formation of the adduct of Pb&lt;sub&gt;2&lt;/sub&gt; with dimethyl sulfoxide (DMSO) and MAI is confirmed at 1,015 cm&lt;sup&gt;-1&lt;/sup&gt; . From the Tauc plot the bandgap energy of TiO2 and Perovskite layers was determined to be 3.52 eV and 2.06 eV respectively. An open-circuit voltage was 0.9057 V and short circuit current density was 12.2185 mA/cm&lt;sup&gt;2&lt;/sup&gt; with a fill factor of 48.05 and power conversion efficiency (PCE) of 5.199%.&lt;/p&gt;

Investigating the Electrocatalytic Oxygen Evolution Reaction of Hydrothermally Synthesized NiFe2O4 Nanoparticles

In this study, nickel ferrite (NiFe2O4) nanoparticles were synthesized using the hydrothermal method at various pH values. The objective was to investigate the influence of pH variation on particle size and electrocatalytic activity. The formation of cubic phase nanoparticles was confirmed through X-ray diffraction (XRD) analysis. To characterize the electrochemical properties, the nickel ferrite nanoparticles were coated onto a stainless steel substrate using the doctor blade technique. The microstructural analysis was conducted using scanning electron microscopy (SEM). The samples were further analyzed using linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS). The average crystallite size, determined from the XRD pattern, was approximately 40 nm. SEM images revealed a conversion from nanoplates to a granular morphology. The synthesized electrode exhibited an overpotential of 392 mV at 10 mA/cm2 and demonstrated good stability for 5 hours. These findings highlight the excellent electrocatalytic activity of nickel ferrite nanoparticles for the oxygen evolution reaction (OER).

Enhancement of synergistic effects of Cu2O@MnO2@NiO Using Sarcophrynium Brachystachys leaf extract for supercapacitor electrode application

In recent times, the global population explosion and growing depletion of fossil fuels have compelled academics and scientists to do extensive research on alternate energy sources and energy storage techniques. A hydrothermal approach was used to create Copper (II) oxide (Cu2O), Manganese oxide (MnO2), Nickel oxide (NiO), and Copper@Manganese@Nickel (Cu2O@MnO2@NiO) oxide composite electrodes. Sarcophrynium Brachystachys leaves extract was used equally as a bolstering mediator. According to the Debye-Scherer equation, the crystallites size of different nanoparticles (NPs) were established to be 29.45, 24.22, 26.33 and 20.24 nm for Cu2O, MnO2, NiO, and Cu2O@MnO2@NiO, respectively, based on X-ray diffraction (XRD) experiments. According to electrochemical examinations, assessed specific capacitances for Cu2O, MnO2, NiO, and Cu2O@MnO2@NiO obtained by cyclic voltammetry (CV) using 1.00 mV/s scan rates are 785, 955, 825 and 1092 F/g, respectively. The obtained results clearly showed that separate metallic oxides specific capacitances compared with composites specific capacitance using Sarcophrynium Brachystachys leaves extract, a biological and natural constituent stands superior. Sarcophrynium Brachystachys leaves extract enhanced the synergistic impact between constituents’ ions via lowering electrode resistances, raising electrode conductivity and improving electrode characteristics.

Characterization of lead dioxide composite electrode and its electrochemical properties

TiO2 nanoparticles, as a typical inert metal oxide, were added into [Formula: see text] plating solutions to prepare Ti/PbO2+nano-TiO2 composite coatings. The effect of TiO2 nanoparticles on the electrodeposition process of PbO2 was investigated by voltammetric studies. The composition, structure and morphology of the obtained composite coatings were characterized by X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), and scanning electron microscopy (SEM), respectively. Cyclic voltammetry was employed to study the effect of nano-TiO2 particles on the PbO2 electrodeposition process. It is found that high doping (2–8 g/L) of TiO2 nanoparticles significantly decreased the crystallite size which can be attributed to a crystallite-refining effect of nano-TiO2 during the electrodeposition of PbO2.

Highly Tuning of Sunlight-Photocatalytic Properties of SnO2 Nanocatalysts: Function of Gd/Fe Dopants

Gd/Fe-SnO2 nanopowders as novel photocatalysts for the active removal of Rose Bengal dye and methyl parathion pesticide were synthesized with a low-cost coprecipitation route. The X-ray diffraction analysis of SnO2, Sn0.96Gd0.02Fe0.02O2 and Sn0.94Gd0.02Fe0.04O2 nanopowders proved the formation of a tetragonal phase of tin oxide with average crystallite sizes in the range of 13–18 nm. The Fourier transform infrared (FTIR) spectra of all samples displayed the characteristic absorption bands of SnO2. The nanopowder of the pure SnO2 sample, as seen in its transmission electron microscope (TEM) image, contains spherical-like particles of variable sizes. The TEM images of the Sn0.96Gd0.02Fe0.02O2 and Sn0.94Gd0.02Fe0.04O2 powders revealed the synthesis of fine spherical nanoparticles. Based on the TEM images, the average particle size of the pure, (Gd, 2 wt% Fe) and (Gd, 4 wt% Fe) codoped SnO2 nanopowders was estimated to be 14, 10 and 12 nm, respectively. After the addition of (Gd, 2 wt% Fe) and (Gd, 4 wt% Fe) to the SnO2 structure, the band gap energy of SnO2 was reduced from 3.4 eV to 2.88 and 2.82 eV, respectively. Significantly, the Sn0.96Gd0.02Fe0.02O2 nanocatalyst exhibited a high removal efficiency of 98 and 96% for Rose Bengal dye and methyl parathion pesticide after activation by sunlight for 35 and 48 min, respectively. Furthermore, this catalyst has shown perfect mineralization as well as high stability properties for the treatment of Rose Bengal dye and methyl parathion pesticide. These results suggest the suitability of the Sn0.96Gd0.02Fe0.02O2 nanocatalyst for the treatment of agriculture and industrial effluent under sunlight light energy.

Copper oxide nanoparticles modified electrodes for high-sensitivity detection of uric acid in athletes

This study introduces an innovative electrochemical sensor leveraging copper oxide nanoparticles for detecting uric acid levels in athletes with enhanced sensitivity and selectivity. Employing a novel synthesis protocol, uniform copper oxide nanoparticles were integrated into a chitosan-glutathione biogel matrix, creating a high-performance sensing electrode. The nanoparticles were extensively characterized using XRD, SEM, FTIR, and XPS techniques, confirming their crystalline structure, morphology, and purity. The average crystallite size was determined to be 18 nm. Electrochemical evaluation of the sensor using cyclic voltammetry and electrochemical impedance spectroscopy revealed significantly improved electron transfer kinetics and catalytic activity towards uric acid oxidation. The sensor exhibited a wide linear detection range from 1 μM to 1.2 mM, encompassing both physiological and pathological uric acid levels. Notably, the limit of detection was found to be 0.27 μM, surpassing the performance of most existing metal oxide based uric acid sensors. The sensor also demonstrated excellent anti-interference capability against commonly coexisting species in biological fluids. Furthermore, the practical applicability of the sensor was validated by successfully determining uric acid concentrations in human serum, plasma, and sweat samples, with impressive recovery rates ranging from 96% to 102%. The stability, reproducibility, and cost-effectiveness of the developed sensor make it a promising tool for routine health monitoring and early intervention in athletes, facilitating personalized training and preventing complications associated with uric acid imbalances. The present work offers a significant advancement in non-invasive, reliable, and efficient assessment of uric acid, with potential for widespread implementation in sports medicine and general healthcare.

Controlling the physical properties of Ni1-xMnxFe2O4 multiferroic by the enhancement of ferroelectric phase through the increase of Mn content

The nanoparticles of the spinel ferrite system Ni1-xMnxFe2O4 with x = 0.0, 0.2, 0.4, 0.6, 0.8 and 1.0 were prepared using the auto combustion flash method technique, by using the nitrates as cations source and urea as a fuel agent for combustion. The XRD pattern validates the formation of cubic spinel structure of Ni1-xMnxFe2O4 nanoparticles and traces of hematite phase. By increasing the annealing temperature, the lattice parameter and crystallite size were increased. At various frequencies, the dielectric properties and initial permeability were measured as a function of temperature. The DC resistivity was found to have a linear relationship with temperature, with two regions and one break point at Curie temperature (TC). SEM and TEM analyses are used to investigate the morphology of the samples, as well as the size and shape of the crystallites. The samples' morphology revealed the formation of a uniform and spherical structural distribution. The material transfer to multiferroic at high Mn content accordingly the ferroelectric and ferrimagnetic properties appear, which give the ability of the material to become magnetoelectric material.

Effect of thickness on properties of La-doped Zinc Blende/Wurtzite ZnO thin films prepared by spray pyrolysis

Abstract Thin films of ZnO doped with 3wt% Lanthanum were deposited on glass substrates using spray pyrolysis for varying thicknesses. The impact of thickness on the physical properties of the films was investigated using various techniques. XRD results revealed the formation of a mixture of two phases, cubic Zinc Blende (ZB) and hexagonal Wurtzite (WU), with their ratios changing based on film thickness. Crystallite size measurements indicated that the cubic phase granules remained stable at 14.6 nm up to a thickness of 719 nm, decreasing to 14 nm at 846 nm, while the crystallite size of the hexagonal phase increased to 18 nm at 846 nm. FE-SEM images showed changes in surface morphology with increasing thickness, and EDX analysis demonstrated a consistent La/Zn ratio across all film thicknesses. The refractive index exhibited a shift from normal to abnormal dispersion when the thickness exceeded 719 nm, and the high-frequency dielectric constant decreased from 3.2 to 2.91 as thickness increased. Additionally, optical band gaps ranged from a minimum of 3.19 eV at 719 nm thickness to a maximum of 3.23 eV at 846 nm thickness. The study examined the effectiveness of the deposited films in blocking UV light with a wavelength of 365 nm. It was discovered that the decay time significantly decreased to 143s at a thickness of 661 nm, compared to longer times observed at other thicknesses.&amp;#xD;

Uncovering the potential of industrial waste: turning discarded resources into sustainable advanced materials

To identify solutions for utilizing industrial wastes (slag, sludge, fly ash, and bottom ash) in the development of pro-environmental systems, this paper reviews existing literature and explores material characterization methods. A review analysis was conducted to uncover their potential, and it was found that many utilizations can be made to recycle them into sustainable materials. Structure characterization, optical-dielectric function, and morphology analysis were analyzed to confirm the recent review. Structural properties are represented by crystallite size and crystallinity, where nickel slag shows the smallest distribution (55 ± 10) nm with the highest crystallinity (25.42%), indicating its association with uniformity of response to external disturbances and micro-structural stability. From the analysis of optical and dielectric functions via Kramers Kronig relation, the widening of ∆(LO−TO) was shown by fly ash and slag indicating stable bonding suitable as x-ray shielding and sensor, while high electron loss functions were shown by sludge and bottom ash indicating high potential electronic transition performance. Based on their chemical and physical properties, these industrial wastes are not limited as construction materials and can even be upgraded to more advanced development materials.

Thickness dependence of the room-temperature ethanol sensor properties of Cu2O polycrystalline films

This study investigates the fabrication process of copper thin films via thermal evaporation, with precise control over film thickness achieved through Z-position adjustment. Analysis of the as-fabricated copper films reveals a discernible relationship between grain size (〈D〉) and Z-position, characterized by a phenomenological equation 〈D〉XRDn(Z)=〈D〉0n1+32rZ2+158rZ4 , which is further supported by a growth exponent (n) of 0.41 obtained from the analysis. This value aligns well with findings in the literature concerning the growth of copper films, thus underlining the validity and reliability of our experimental outcomes. The resulting crystallites, ranging in size from 20 to 26 nm, exhibit a resistivity within the range of 3.3–4.6 μΩ · cm. Upon thermal annealing at 200 °C, cuprite Cu2O thin films are produced, demonstrating crystallite sizes ranging from ∼9 to ∼24 nm with increasing film thickness. The observed monotonic reduction in Cu2O crystallites relative to film thickness is attributed to a recrystallization process, indicating amorphization when oxygen atoms are introduced, followed by the nucleation and growth of newly formed copper oxide phase. Changes in the optical bandgap of the Cu2O films, ranging from 2.31 to 2.07 eV, are attributed mainly to the quantum confinement effect, particularly important in Cu2O with size close than the Bohr exciton diameter (5 nm) of the Cu2O. Additionally, correlations between refractive index and extinction coefficient with film thickness are observed, notably a linear relationship between refractive index and charge carrier density. Electrical measurements confirm the presence of a p-type semiconductor with carrier concentrations of ∼1014 cm−3, showing a slight decrease with film thickness. This phenomenon is likely attributed to escalating film roughness, which introduces supplementary scattering mechanisms for charge carriers, leading to a resistivity increase, especially as the roughness approaches or surpasses the mean free path of charge carriers (8.61 nm). Moreover, ab-initio calculations on the Cu2O crystalline phase to investigate the impact of hydrostatic strain on its electronic and optical properties was conducted. We believe that our findings provide crucial insights that support the elucidation of the experimental results. Notably, thinner cuprite films exhibit heightened sensitivity to ethanol gas at room temperature, indicating potential for highly responsive gas sensors, particularly for ethanol breath testing, with significant implications for portable device applications.

Nanostructuring of an additively manufactured CoCrFeNi multi-principal element alloy using severe plastic deformation: Comparison of two materials processed by different laser scan speeds

Experiments were conducted to reveal the refinement of the microstructure and the evolution of the hardness of an additively manufactured (AM) CoCrFeNi multi-principal element alloy (MPEA) processed by severe plastic deformation (SPD) using high pressure torsion (HPT) technique. AM was carried out by laser powder bed fusion (L-PBF) technique at two different laser scan speeds. The as-built alloys for both laser scan speeds have a single-phase face-centered cubic (fcc) structure with <110> fiber texture parallel to the building direction. X-ray line profile analysis (XLPA) revealed that the dislocation density was considerably high even in the AM-processed state before HPT (3 × 1014 m−2) which increased by two orders of magnitude during HPT. The saturation of the lattice defects (dislocation density and twin fault probability) as well as the crystallite size occurred at a shear strain of about 10 during HPT. In both AM-processed alloys, <111> fiber texture developed parallel to the normal of the HPT-processed disks. For both laser scan speeds, the initial grain size in the AM-processed samples was refined from 70 to 90 μm to the nanocrystalline regime after 10 turns of HPT. Additionally, nanotwins formed with a probability of about 3 %. The initial hardness of the AM-processed MPEA samples for both laser scan speeds was 2700–2800 MPa, which is superior to that of CoCrFeNi produced by casting (about 1380 MPa). This can be explained by the high dislocation density in the AM-processed specimens. The formation of nanostructure with high lattice defect density during HPT resulted in a very high hardness value of about 5500 MPa in the AM-processed CoCrFeNi MPEA samples for both laser scan speeds.

Tailoring perovskite ceramics for improved structure, vibrational behaviors and radiation protection: The role of lanthanum in PbTiO3

This study investigates the characteristics of lanthanum (La)-doped lead titanate (PbLaxTi(1-3x/4)O3 where, x = 0.0, 0.02, 0.04, 0.06, 0.08, and 0.1), a type of perovskite ceramic. It specifically focuses on analyzing its structure, vibrational properties, and efficacy in shielding against radiation. The prepared samples are investigated by X-ray diffraction (XRD), which clarified that the small doping of La (x ≤ 0.06) produced the required phase, and increasing the La doping (x > 0.06) produced nonrequired phases (secondary phase). Also, increasing the La doping converted the crystal symmetry from tetragonal to cubic, which was confirmed by the tetragonality raio (c/a) calculations. Also, the samples are investigated by Fourier transform infrared (FTIR) spectroscopy to confirm the XRD results. Transmission electron microscopy (TEM) examination clarified that the prepared samples were in the nanoscale range with a maximum crystallite size value of around 70 nm. In addition, the shielding effectiveness of all the prepared samples was theoretically evaluated using the Phy-X/PDS program by considering characteristics such as the linear attenuation coefficient (GLAC), mean free path (GMFP), transmission factor (TF), and radiation protection efficiency (RPE). Increasing the La concentration increases the theoretical density to 4.98 gm/cm3 at x = 0.1, leading to low TF and GMFP values and high GLAC values. This produces samples with high attenuation to radiation and high shielding effectiveness.

Growth of variable aspect ratio ZnO nanorods by hydrothermal technique

Zinc oxide (ZnO) nanorods were successfully prepared by hydrothermal process. The influence of the solution temperature on the ZnO nanorods aspect ratio is investigated in the present work. The x-ray diffraction (XRD) and scanning electron microscopy (SEM) results and analysis reveal the formation of ZnO nanorods owing hexagonal Wurtzite structure with preferential orientation along the c-axis. We found that the solution temperature is a key parameter controlling the aspect ratio of the formed ZnO nanorods. The later increases linearly with the preparation temperature. The rod length is thermally activated with an activation energy of 0.48 eV, which corresponds to the activation energy of the reaction forming ZnO, indicating that the nanorods growth is controlled by the surface reaction rather than by mass transport. While, the rods diameter is reduced with increasing temperature, its activation energy of 0.23 eV is equal to the species diffusion activation energy in the solution and to the crystallite size activation energy suggesting, thereafter that the rod diameter variation is controlled by the nucleation dynamic.

Nanocomposite marvels: Miniaturized high bandwidth microstrip patch antenna for X-band applications

Zinc aluminate (ZnAl2O4) is widely recognized as a ceramic in high demand across various microwave applications. Furthermore, blending dielectric materials with ZnAl2O4 has demonstrated improvements in its dielectric properties, offering promising potential for advancing microstrip patch antenna technology. This paper presents the fabrication and characterization of a sol-gel composite nanoparticle consisting of titanium dioxide (TiO2) and zinc aluminate (ZnAl2O4) for use in a microstrip patch antenna designed for X-band applications. The composite nanoparticle, with a molecular composition of xTiO2(1-x)ZnAl2O4 where x = 8 %, was investigated using X-ray diffraction (XRD), revealing dominant peaks corresponding to ZnAl2O4 and TiO2 with a calculated crystallite size of 16.9 nm. Fourier transform infrared spectroscopy (FTIR), field-emission scanning electron microscopy (FESEM), and energy dispersive spectroscopy (EDS) were employed to assess functional groups, morphology, and elemental composition of the nanoparticles. The dielectric properties of the nanoparticles, characterized by a dielectric permittivity of 20.2 and a dielectric loss of 0.19, were measured using an LCR meter. These nanoparticles were utilized to fabricate a prototype patch antenna, exhibiting promising performance in both simulated and measured results. The fabricated patch antenna operated at 8.51/8.49 GHz with a return loss (RL) of − 25.94/−19.97 dB, featuring an enhanced bandwidth of 2.62/2.87 GHz and a voltage standing wave ratio (VSWR) below 2. Additionally, the antenna demonstrated a gain of 2.14, directivity of 3.58, and radiation efficiency of 59.7 %, making it suitable for X-band applications.

A comparative approach for estimating microstructural characteristics of BaTi1−xZrxO3 (0.0 ≤ x ≤ 0.3) nanoparticles via X-ray diffraction patterns

AbstractBarium titanate materials are currently a special topic for scientific research due to their effective technological applications. The tetragonal BaTi1-xZrxO3 (0.0 ≤ x ≤ 0.3) nanoparticles (NPs) were synthesized using a modified citrate technique. The current work provides a comparative approach for the calculation of crystallite size, stress, strain, and elastic characteristics based on X-ray diffraction (XRD) patterns. Various models have been developed to analyze XRD data; these models differ in their assumptions, mathematical approaches, and the type of information they provide. The Scherrer model ignores lattice micro-structures that develop in nanostructures, such as intrinsic strain. To overcome such drawbacks, three Williamson-Hall models, (the uniform deformation model (UDM)), the uniform stress deformation model (USDM), and the uniform deformation energy density model (UDEDM) have been discussed. According to the USDM model, with increasing Zr ion concentrations, interplanar space increases, causing a drop in Young’s modulus. All the previous approaches take into account the diffraction angle (2θ)-dependent peak broadening, which is thought to represent a combination of size and strain-driven induced broadening. Graphical Abstract

Efficient removal of crystal violet dye from water using zinc ferrite-polyaniline nanocomposites.

Nanomaterials are widely employed in wastewater treatment, among which nanoferrites and their composites hold significant prominence. This study adopts a green approach to synthesize zinc ferrite nanoparticles, subsequently integrating them with polyaniline (PANI) to fabricate the ZnFe2O4-PANI nanocomposite. Characterization of the prepared ZnFe2O4-PANI nanocomposite was conducted using X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopic (SEM) techniques. Using Scherrer's equation, the crystallite size of the synthesized zinc ferrite nanoparticles was found to be 17.67nm. SEM micrographs of the ZnFe2O4-PANI nanocomposite revealed that in situ polymerization of ZnFe2O4 with polyaniline transforms the amorphous surface morphology of the polymer into a homogeneous nanoparticle structure. The adsorption of crystal violet (CV) dye onto the surface of the ZnFe2O4-PANI nanocomposite depends on pH, adsorbent dosage, temperature, concentration levels and duration. The Langmuir adsorption model fitted the data well, indicating adherence to a pseudo-second-order kinetic pattern. Thermodynamic values ΔG°, ΔH° and ΔS° indicated that the adsorption process occurred spontaneously. Advantages and disadvantages of the technique have also been highlighted. Mechanism of adsorption is discussed. From the obtained results, it is evident that the ZnFe2O4-PANI nanocomposite holds promise as a sorbent for the removal of dye from wastewater.

Physicochemical Characterization of Hydroxyapatite Hybrids with Meloxicam for Dissolution Rate Improvement

Organic–inorganic hybrids represent a good solution to improve the solubility and dissolution rates of poorly soluble drugs whose number has been increasing in the last few years. One of the most diffused inorganic matrices is hydroxyapatite (HAP), which is a biocompatible and osteoconductive material. However, the understanding of the hybrids’ functioning mechanisms is in many cases limited; thus, thorough physicochemical characterizations are needed. In the present paper, we prepared hybrids of pure and Mg-doped hydroxyapatite with meloxicam, a drug pertaining to the Biopharmaceutical Classification System (BCS) class II, i.e., drugs with low solubility and high permeability. The hybrids’ formation was demonstrated by FT-IR, which suggested electrostatic interactions between HAP and drug. The substitution of Mg in the HAP structure mainly produced a structural disorder and a reduction in crystallite sizes. The surface area of HAP increased after Mg doping from 82 to 103 m2g−1 as well as the pore volume, justifying the slightly high drug amount adsorbed by the Mg hybrid. Notwithstanding the low drug loading on the hybrids, the solubility, dissolution profiles and wettability markedly improved with respect to the drug alone, particularly for the Mg doped one, which was probably due to the main distribution of the drug on the HAP surface.

Biogas dry reforming over Li–Ni–Al LDH-derived catalysts

Biogas dry reforming or dry reforming of methane (DRM) is an alternative to produce hydrogen, in the context of development of sustainable routes for energy production, since this route uses CH4 and CO2, two greenhouse gases as reactants. However, the deactivation of catalysts due to carbon deposition and sintering is the main drawback of this reaction. In this work, with the aim of minimizing carbon formation and sintering during DRM, the effect of lithium as a promoter in catalysts Ni–Al derived from layered double hydroxides was investigated. The catalysts were prepared by co-precipitation and characterized by different techniques: BET surface area (SBET), X-ray diffraction (XRD), temperature-programmed reduction (TPR), CO2 and H2 temperature-programmed desorption (CO2-TPD and H2-TPD), Scanning Electron Microscopy (SEM-EDS), temperature-programmed oxidation (TPO). The catalytic tests were carried out in a fixed bed reactor using a synthetic biogas (60% CH4 and 40% CO2) in the temperature range of 500–750 °C. The incorporation of Li into the Ni–Al-LDH changed the reducibility and basicity of the catalysts. The Li2 sample containing an intermediary amount of Li (5 wt%) showed the highest reduction temperature and highest density of basic sites, which resulted in the smallest Ni crystallite size before and after the reactions. As a result, this catalyst presented the greater resistance to sintering and a lower rate of carbon produced. For the reaction carried out at 700 °C, only the Li2 catalyst remaining active during the test and reaching a maximum of 80% and a final CH4 conversion of 54% after 480 min of reaction, whereas CO2 conversion was higher than 90%. All other samples deactivated at different rates due to carbon deposition and sintering.