X-ray Diffraction Spectroscopy Research Articles

Design and characterization of borosilicate glass modified with TiO2 for enhanced optical and radiation shielding applications

This work investigates the potential of borosilicate glass doped with titanium dioxide (TiO2) for radiation shielding applications. The study explored the impact of varying TiO2 concentrations on the glass structure, optical properties, and radiation shielding effectiveness. X-ray diffraction (XRD) and Raman spectroscopy confirmed the amorphous nature of the glasses. The addition of TiO2 affected the glass network structure, as evidenced by changes in the Raman spectra and density measurements. UV–Vis spectroscopy revealed a red shift in the absorption edge (416–481 nm) and a decrease in the indirect optical band gap (2.91–2.70 eV) with increasing TiO2 content. The refractive index also increased from 2.54 to 3.54 with TiO2 concentration. The mass attenuation coefficient (MAC) and linear attenuation coefficient (LAC) increased significantly with TiO2 addition, indicating enhanced radiation attenuation capability. The inclusion of TiO2 reduced the half-value layer (HVL), tenth-value layer (TVL), and mean free path (MFP), while increasing the effective atomic number (Zeff). The effective electron density (Neff) and effective conductivity (Ceff) showed a slight increase with TiO2 content. Energy build-up factors (EBF and EABF) indicated a higher rate of radiation intensity increase and energy absorption within the glass due to the presence of TiO2. Finally, the incorporation of TiO2 into borosilicate glass offered a promising approach to developing improved optical and radiation shielding glasses.

Over 10% efficient Cu2ZnSn(S, Se)4 Thin-Film cells prepared by aluminium doping

Cu2ZnSn(S,Se)4(CZTSSe) solar cell is of excellent development tendency because of lower pollution and outstanding power conversion efficiency(PCE). Yet, current PCE of CZTSSe is limited because of a high open-circuit voltage deficit, primarily put down to severe band tailing and carrier recombination. In this paper, absorber films were obtained by solution method and the influences of different aluminum doping concentrations on the properties of CZTSSe thin film cell were studied. Analysis about X-ray diffraction (XRD) and Raman spectroscopy confirms which Al has incorporated into CZTSSe thin film lattice and replaced Sn. Hall effect measurements reveal the improvement of carrier concentration on thin film absorber layer attribute to the formation of AlSn acceptor defects. Furthermore, X-ray photoelectron spectroscopy (XPS) reveals that Al enter into the CZTSSe lattice and Al is in the appropriate state of + 3 valence without generating additional harmful defects. More important, the generation of deep energy level defects and defect clusters associated with Sn were suppressed by replacing Sn with Al. Finally, the photovoltaic performance of different Al doped CZTSSe cells were characterized by conducting J-V and external quantum efficiency (EQE) tests. Remarkably, the CZTSSe solar cell with PCE as high as 10.59 % is obtained under a doping level of 6 % Al, which has an open circuit voltage of 522 mv. Compared with reference CZTSSe solar cells with an efficiency of 7.29 %, which indicates with improvement of 45 % in efficiency. Consequently, Al doping process is considered as a prospective tactic to elevate the PCE of CZTSSe solar cells.

Ligand Noninnocence in β-Diketiminate and β-Diketimine Copper Complexes.

Metal-ligand cooperative systems have a long precedent in catalysis, with the classification depending on the site of substrate bond cleavage and formation and on redox state changes. Recently, our group reported the participation of a β-diketiminate ligand in chemical bonding to heterocumulenes such as CO2 and CS2 by tricopper complexes, leading to cooperative catalysis. Herein, we report the reactivity of these copper clusters, [Cu3EL]- (E = S, Se; L = tris(β-diketiminate) cyclophane ligand), toward other electrophiles, viz. alkyl halides and Brønsted acids. We identified a family of ligand-functionalized complexes, Cu3EL (R) (R = primary alkyls), and a series of disubstituted products, Cu3EL (R)2, through single-crystal X-ray diffraction, mass spectrometry, and infrared and UV-visible spectroscopy. As part of mechanistic studies on these alkylation reactions, we evaluated the acid-base reactivity of these complexes and the influence of the backbone substitution on the reduction potential. Implications of these findings for ligand noninnocence and the relevance of the metal core as a cofactor for the ligand's reactivity are discussed.

Engineering the S-scheme heterojunction between NiFeAl - LDH and BiOCOOH nanoflower by constructing an interfacial electric field for efficient degradation of levofloxacin under visible light

The antibiotic levofloxacin (LVF), utilized across the world during the COVID-19 pandemic, presents a notable concern in environmental safety owing to its deposition in water bodies. This work reports the engineering of S-scheme heterojunction, NiFeAl LDH coupled with BiOCOOH nanoflower by constructing an interfacial electric field for efficient degradation of LVF under visible light. The scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis reveal the uniform decoration of NiFeAl LDH flakes over flowers like BiOCOOH and the high crystallinity is confirmed with SAED pattern distribution. The construction of an interfacial electric field was confirmed by X-ray photoelectron microscope (XPS) analysis. The X-ray diffraction (XRD), XPS, and Raman spectroscopy studies were conducted to confirm the purity and chemical bonding nature of the BiOCOOH-NiFeAl LDH nanocatalyst (NFB NCs). The band gap of materials was calculated to be 3.38 and 2.03 eV for BiOCOOH and NiFeAl LDH respectively. The NFB NCs showed remarkable performance of 95.2 % than its pristine BiOCOOH (35.4 %) and NiFeAl LDH (18 %). ESR and scavenging studies identified the major involvement of •OH, O2•- and h+ in the process. The intermediates formed during the degradation were examined by using GC–MS and a possible degradation pathway was proposed. Furthermore, the toxicity analysis using the ECOSAR program demonstrates NFB NCs safety level for extensive wastewater treatment. The stability of the NCs over six cycles and magnetic removal properties showcased their potential for large-scale wastewater treatment applications. This comprehensive study highlights the importance of LDH in advancing photocatalytic materials for environmental remediation and paves a way for manufacturing innovation.

Green synthesis of ZnO nanoparticles and biological applications as broad-spectrum bactericidal, antibiofilm effects and biocompatibility studies on Zebrafish embryo

This work generated zinc oxide nanoparticles (ZnO NPs) using Ocimum tenuiflorum in an inexpensive and environmentally friendly manner. The generated ZnO NPs were analysed using Ultra visible spectroscopy (UV–Vis), Fourier transformed infrared spectroscopy (FTIR), Scanning electron microscopy-Energy X-ray diffraction spectroscopy (SEM-EDX), Transmission electron microscopy (TEM), and X-ray diffraction (XRD). Bio-synthesized ZnO NPs showed UV–Visible absorbance maxima at 290 nm, indicating bio reduction and stability. The DRS spectra revealed a straight band gap value of 3.24 eV. Alcohols, alkanes, phenols, and amines in FTIR may contain reduced and capped zinc ions. Crystalline ZnO nanoparticles were verified by XRD. Biosynthesized ZnO NPs were exhibited in spherical and 5–35.49 nm in size by FESEM and TEM. EDX confirmed NPs zinc elemental signatures. Antibacterial properties showed that ZnO NPs effectively inhibited gram (+ve) and gram (−ve) pathogens, including E. coli (20.0 ± 0.8 mm), E. faecalis (20.0 ± 0.5 mm), S. aureus (18.01 ± 1.2 mm), and S. mutans (17.5 ± 1.0 mm). This study shows that biosynthesized ZnO NPs inhibit biofilm growth by 0.198–1.431 O.D values (Optical density). Antibiofilm inhibition was concentration-dependent. Nanoparticles proved effective against E. coli, S. mutans, S. aureus, and E. faecalis with MICs of 15 and 25 µg/mL. Time-dependent death kinetic studies indicated that 8–12 h ZnO NPs killed all bacteria. Also, ZnO NPs had low harmful effects on zebrafish eggs at doses upto 1 mg/mL. In summary, the production of green ZnO NPs offers a sustainable and biocompatible approach that is well-suited for various biological applications.

On the microstructure, corrosion behavior and surface films of the multi-principal element alloy CrNiTiV

A multi-principal element alloy consisting of equi-atomic concentrations of Cr, Ni, Ti, and V, was produced by arc melting. The CrNiTiV alloy was characterized using scanning electron microscopy, energy-dispersive X-ray spectroscopy, X-ray diffraction, and scanning transmission electron spectroscopy (STEM), revealing a complex microstructure containing five phases. The corrosion performance of the alloy was evaluated with cyclic potentiodynamic polarization tests, indicating a low corrosion current density, a high breakdown potential and high repassivation potential. X-ray photoelectron spectroscopy and STEM were carried out after constant immersion in 0.6 M NaCl solution, revealing the passive (surface) film for each of the five phases. The Cr and V dominant phase consisted of an oxidized Cr/V-rich surface film, while the remaining four Ti-containing phases were predominantly TiO2-rich surface films. Ni enrichment and Ti deficiency were observed at the metal/oxide interface in certain Ti-containing phases.

Tailoring photocatalytic performance: Lanthanum doping in nickel oxide for efficient degradation of some industrial cationic dyes in visible light radiation

Metal oxide nanoparticles have emerged as an important component in heterogeneous photocatalysis, which uses light-induced reactions on the surface of a catalyst to drive chemical transformations. The improved photocatalytic activity of lanthanum-doped metal oxide nanoparticles has been the subject of research due to their special qualities, which include enhanced photocatalytic performance, stability and absorption of visible light. This study involves co-precipitation approach to synthesize nickel oxide nanoparticles and nickel oxide nanoparticles doped with lanthanum. The nanoparticles were determined using UV-Visible absorption spectrophotometry, X-ray diffraction spectroscopy, Energy-disperse spectroscopy, Photoluminescence spectroscopy and Field emission scanning electron microscopy. For the photodegradation of malachite green and rhodamine B dyes, synthesized nanoparticles were employed as photocatalysts. Compared to pure NiO, the photochemical activity of 4 % Lanthanum-doped NiO was higher. The degrading efficiency of 4 % La-doped NiO is 89 % effective towards rhodamine B and 87 % for malachite green. In addition, entrapment was done to identify primary active species responsible for photocatalytic activity. The present study likely provides new insights and novelty into the photocatalytic mechanisms at play, including how lanthanum doping affects the generation and dynamics of reactive oxygen species (ROS) like hydroxyl radicals and superoxide anions, which are responsible for the breakdown of dye molecules.

Effect of acid soak treatment of the precursor on the structure and properties of polypropylene-based carbon fibers

Polyolefin fibers have received wide attention as the precursor for low-cost carbon fiber, and cross-linking of linear polyolefin by strong acid has been proven to be an effective way to stabilize the precursor fiber prior to carbonization. However, the conventional temperature used in sulfonation process is too high and could result in severe decomposition of the linear chain of the polymer, which further deteriorated the mechanical properties of the as-prepared carbon fiber. Thus, reducing the duration of sulfonation process operated at high temperature may alleviate the degradation behavior, conferring the polyolefin-based carbon fibers with better performance. In this paper, polypropylene (PP) fibers were soaked in sulfuric acid at 50 °C–90 °C, before the conventional preparation protocol of PP-based carbon fiber. The structural evolution from PP to carbon fiber were characterized by Differential scanning calorimetry (DSC), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and Raman spectroscopy. The mechanical and conductive properties of carbonized fibers where further measured. The results showed that the soak in sulfuric acid resulted in swelling of PP fibers in diameter direction, as well as reducing the crystallinity of the fibers, both of which were physical transformation, and could be easily controlled by soak temperature. The subsequent sulfonation at conventional temperature was fastened for the soaked PP fibers, and the duration of sufficient sulfonation were almost reduced by half. The obtained carbon fibers exhibited better thermal conductivity and mechanical properties, which were enhanced by 25 % and 40 %, respectively, compared with that without soak pretreatment.

Photocatalytic performance of Soot/TiO2 nanocomposite against toxic dye

Nowadays, composing semiconductors with carbon structures to enhance their optical properties shows huge interest as a nanophotocatalyst for trending applications (i.e., photodegrading pollutants). In this study, TiO2 and soot/TiO2 nanocomposites were prepared via a one-step sol-gel assisted hydrothermal method, using a temperature of 220 °C and a reaction time of 6 h. Characterization by X-ray diffraction and Raman spectroscopy confirmed that the resulting TiO2 and soot/TiO2 materials exhibited a pure anatase crystal phase, without the presence of other TiO2 polymorphs. Soot composition on TiO2 showed enhanced photocatalysis properties, such as a lower combination rate of electron-hole pairs than pure TiO2. Crystal violet (CV) was applied as a pollutant model to examine the photocatalytic degradation of synthesized TiO2 and soot/TiO2. The photodegradation experiments of CV dye in its aqueous media by UV light interaction showed 26.63 % and 89.09 % in the presence of TiO2 and soot/TiO2 nanocomposite, respectively. In the basic media (pH 11), maximum photodegradation (97.95 %) is attained when 0.004 g of Photocatalyst (soot/TiO2) is used. Using the recycled photocatalyst, the dye's photodegradation efficiency remained high throughout the reusability cycles, even after four consecutive cycles.

Combining electron transfer, spin crossover, and redox properties in metal-organic frameworks

Hofmann coordination polymers (CPs) that couple the well-studied spin transition of the FeII central ion with electron-responsive ligands provide an innovative strategy toward multifunctional metal-organic frameworks (MOFs). Here, we developed a 2D planar network consisting of metal-cyanide-metal sheets in an unusual coordination mode, brought about by infinitely π-stacked redox-active bipyridinium derivatives as axial ligands. The obtained family of materials show vivid thermochromism attributed to electron transfer and/or electronic spin state change processes that can occur either independently or concomitantly. Importantly, the redox activity of the ligands within the structure leads to the quasi-reversible electrochemical reduction reaction on a spin-crossover complex at solid state. These observations have been confirmed via temperature-dependent single-crystal X-ray diffraction, magnetic measurements, Mössbauer, EPR, optical and vibrational spectroscopies as well as quantum chemical calculations.

HYDROTHERMALLY DEVELOPED TITANIUM DIOXIDE AND EUROPIUM-DOPED COMPOSITE MATERIALS FOR PHOTODEGRADATION APPLICATIONS

Metal oxide nanocomposites are a critical element in nanoscale technology. Because of their many uses, a great deal of study has involved photocatalytic materials. These photocatalytic degradation characteristics also included applications like solar-cell applications. Waste­water management was included in the photodegradation property. The following study explored the development of europium tungstate nanocomposites with titanium dioxide and how they can be used in photocatalytic applications. The synthesis was conducted using the hydrothermal method and is characterized by Fourier-transform infrared spectroscopy, X-ray diffraction spectroscopy, scanning electron microscopy, and energy-dispersive spectroscopy. Application experiments were conducted using four distinct dyes, namely methyl orange, methylene blue, congo red and methyl red. The photodegradation experiments were conducted using visible light emitted by a tungsten-filament lamp. Methylene blue and methyl orange degraded to 20 % and 35 % after 1 hour respectively. After 90 min, the degradation of methylene blue went down to 15 % and congo red degraded down to 9 %. With the experiment conducted, the sample showed that it had a relatively higher photodegradation property with the dyes used. The results show that the compound had better reaction with these dyes, with a degradation down to 10 %.

Investigating the impact of various etching agents on Ti3C2Tx MXene synthesis for electrochemical energy conversion

MXenes represent a revolutionary class of two-dimensional (2D) materials that have garnered significant attention due to their unique properties, including excellent electrical conductivity, and remarkable mechanical strength. This study investigates the influence of different etching agents on the synthesis of MXenes for electrochemical energy conversion applications, particularly in methanol oxidation reactions (MOR). Morphological characterization, particle distribution and sizing, elemental analysis, and surface chemistry assessments were conducted using field emission scanning electron microscopy (FESEM), elemental mapping, transmission electron microscopy (TEM), x-ray diffraction (XRD), and x-ray photoelectron spectroscopy (XPS). Electrochemical techniques such as cyclic voltammetry (CV), electrochemical active surface area (ECSA), Tafel analysis, electrochemical impedance spectroscopy (EIS), and long-term stability assessment were employed. The study reveals that PtRu/MXene synthesized with the FeF3/HCl etching route exhibits the highest ECSA value and peak current density, being 12.3 times and 3.63 times higher than those achieved via the LiF/HCl etching route. The kinetic rate, tolerance to catalyst poisoning and long-term stability also show the better results for this etching route. These findings suggest promising potential for PtRu/MXene_FeF3/HCl as an effective anodic electrocatalyst in direct methanol fuel cell (DMFC) applications.

Flow-Xl: a new facility for the analysis of crystallization in flow systems.

Characterization of crystallization processes in situ is of great importance to furthering knowledge of how nucleation and growth processes direct the assembly of organic and inorganic materials in solution and, critically, understanding the influence that these processes have on the final physico-chemical properties of the resulting solid form. With careful specification and design, as demonstrated here, it is now possible to bring combined X-ray diffraction and Raman spectroscopy, coupled to a range of fully integrated segmented and continuous flow platforms, to the laboratory environment for in situ data acquisition for timescales of the order of seconds. The facility used here (Flow-Xl) houses a diffractometer with a micro-focus Cu Kα rotating anode X-ray source and a 2D hybrid photon-counting detector, together with a Raman spectrometer with 532 and 785 nm lasers. An overview of the diffractometer and spectrometer setup is given, and current sample environments for flow crystallization are described. Commissioning experiments highlight the sensitivity of the two instruments for time-resolved in situ data collection of samples in flow. Finally, an example case study to monitor the batch crystallization of sodium sulfate from aqueous solution, by tracking both the solute and solution phase species as a function of time, highlights the applicability of such measurements in determining the kinetics associated with crystallization processes. This work illustrates that the Flow-Xl facility provides high-resolution time-resolved in situ structural phase information through diffraction data together with molecular-scale solution data through spectroscopy, which allows crystallization mechanisms and their associated kinetics to be analysed in a laboratory setting.

Solution-Free Melt-Grown CsGeI3 Polycrystals for Lead-Free Perovskite Photovoltaics: Synthesis, Characterization, and Theoretical Insights

Inorganic lead-free metal halide perovskites are being rigorously explored as a substitute for organic lead-based materials for various energy device applications. Germanium as a replacement for lead has been proven to give exemplary results theoretically, and there have been promising results. The current work presents the investigation of CsGeI3 (CGI) polycrystals grown using a solution-free melt-growth technique with low-cost precursors. A soak-ramp profile was designed to synthesize polycrystalline powders, which were evaluated for stability. X-ray diffraction and Raman spectroscopy analysis suggest the formation of CsGeI3 perovskite powders, matching the reported literature. Diffuse reflectance spectroscopy measurements showed the bandgap of the polycrystals to be around 1.6 eV. A prominent photoluminescence peak was obtained at 767 nm. The powders were examined using thermogravimetric analysis to assess the thermal degradation pathways. The as-grown inorganic perovskite polycrystals were relatively stable during storage under ambient conditions. Theoretical studies were also carried out to support the experimental data. Calculations were performed with different approximations, including local density approximation (LDA), generalized gradient approximation (GGA), and Heyd–Scuseria–Ernzerhof (HSE) approximation, out of which the HSE approximation yielded the most accurate results that matched the experimental findings. Moreover, for the CGI device with Ag electrodes simulated using SCAPS-1D software, highest incident photon-to-electron conversion efficiency was observed. The obtained optical and structural properties indicate the suitability of the synthesized CsGeI3 perovskite polycrystals for photovoltaic applications, specifically solar cells and light-emitting diodes.

Rapid pyrolysis of cellulose: Revealing the role of volatile matter and char structure evolution

The complexity of the cellulose structure hinders its energy conversion and utilization. Pyrolysis is not only an independent thermochemical conversion technology but also a necessary stage in the gasification process. The real-time capture of volatile components in cellulose pyrolysis is difficult, and the evolution of char structures is lacking, which is extremely challenging. In this work, elemental analysis, industrial analysis, thermogravimetric analysis, infrared spectroscopy (FTIR), Raman spectroscopy (Raman), and X-ray diffraction spectroscopy (XRD) were used to characterize the raw materials and products. Combined with rapid pyrolysis experiments, the pathways of cellulose pyrolysis volatiles and char structure evolution were explored. Dehydrated sugars are the initial products formed below 350 ℃, which quickly dehydrate to form furan compounds at 400 ℃ and then break CC bonds at 600 ℃ to generate fatty aldehydes, ketones, and carboxylic acids. Biochar generated at low temperatures (<300°C) has strong lipid solubility. An increase in pyrolysis temperature leads to a continuous decrease in the content of H and O in biochar, which destroys its functional groups and physical structure, and ultimately tends to form graphite-type char with aromatic structures. Based on the correlation between the volatile matter release characteristics and the evolution of the semichar structure, a cellulose pyrolysis pathway was established, providing theoretical support for the high-value utilization of cellulose.

Exploring the structural variations and magnetic properties of three hexanuclear dysprosium(III) complexes exhibiting single-molecule magnetism behavior

Three novel hexanuclear DyIII complexes supported by polyhydroxy Schiff-base ligands, [Dy6(hmc)3(μ-acac)2(acac)3(μ3-OH)4(H2O)2]·2MeCN (1·2MeCN), [Dy6K2(hmc)3(μ-CO3)6(μ3-CO3)4(H2O)2]·8MeOH (2·8MeOH) and [Dy6(hmc)3(μ-OAc)6(μ3-OH)3(H2O)3] (3) (H3hmc: 1,5-bis(2-hydroxy-3-methoxybenzylidene)carbonhydrazide), have been prepared and structurally characterized by single-crystal X-ray diffraction, elemental analysis, and IR spectroscopy. Each of the hexanuclear complexes is constructed from triangular Dy3 building blocks, with the six DyIII ions are arranged in three different conformations. The magnetic properties of three dinuclear DyIII complexes have also been investigated (Fig. S2). The frequency-dependent ac susceptibility is indicative of Single-Molecule Magnet behavior without and/or with optimum dc field for complexes 2 and 3.

Nanocomposite-modified nanopores: A promising platform for selective detection of copper ions

This research introduces an innovative platform designed for the selective detection of copper (II) (Cu2+) ions, employing a singular nanopore embedded within a 12 μ m-thick polyethylene terephthalate (PET) membrane. The track-etched nanopore was subsequently modified with nanomaterials in an allylamine hydrochloride (PAH)-modified asymmetric nanopore through electrostatic interactions. The nanomaterials included copper oxide (CuO), graphene oxide (GO), and their composite (GO/CuO), were synthesized using wet chemistry, and their structures and optical properties were thoroughly investigated using x-ray diffraction and diffuse reflectance spectroscopy. In the distinctive feature of the platform, Cu2+ ions gain access to coordination sites across a broad surface covered by the immobilized nanomaterials, facilitating effective binding. The selective response of GO/CuO modified pores towards Cu2+ ions was notably observed through ion transportation (I –V) studies, surpassing the response of unmodified nanopores and those modified with CuO alone. This selective behavior was demonstrated in the presence of various monovalent and divalent competing ions. Quantitative assessment of I –V studies was conducted by evaluating the intrinsic rectification ratio of asymmetric nanopores, providing a robust measure of platform's efficacy. Furthermore, we identified the optimal pH for detecting Cu2+ ions as 7, enhancing the specificity and accuracy of our method.

Influence of Mg doping on structure and optical properties of red-emitting phosphor Li2TiO3:Mn4+

Li2TiO3:Mn4+ has been previously identified as a potential candidate to replace commercial red-emitting Eu2+-activated phosphors. Its luminescent efficiency is limited by the presence of defects and the sensitivity of Mn4+ to redox processes. A series of co-doped Li2TiO3: x Mg2+, 0.01 Mn4+ samples were prepared to gain insight on the effect of electron doping on the structure and photoluminescent properties, through characterization by powder X-ray diffraction, elemental analysis, and optical spectroscopy. As Mg2+ substitutes for Li+, the ordered arrangement of cations within the honeycomb layers in the parent structure (Li2SnO3-type, an ordered derivative of rocksalt) gradually transforms to a more disordered arrangement. The increased cation site disorder leads to less intense and broader emission peaks as well as lower quantum yields.

Biogenic Synthesis Based on Cuprous Oxide Nanoparticles Using Eucalyptus globulus Extracts and Its Effectiveness for Removal of Recalcitrant Compounds

Recalcitrant compounds resulting from anthropogenic activity are a significant environmental challenge, necessitating the development of advanced oxidation processes (AOPs) for effective remediation. This study explores the synthesis of cuprous oxide nanoparticles on cellulose-based paper (Cu2O@CBP) using Eucalyptus globulus leaf extracts, leveraging green synthesis techniques. The scanning electron microscopy (SEM) analysis found the average particle size 64.90 ± 16.76 nm, X-ray diffraction (XRD) and Raman spectroscopy confirm the Cu2O structure in nanoparticles; Fourier-transform infrared spectroscopy (FTIR) suggests the reducing role of phenolic compounds; and ultraviolet–visible diffuse reflectance spectroscopy (UV-Vis DRS) allowed us to determine the band gap (2.73 eV), the energies of the valence band (2.19 eV), and the conduction band (−0.54 eV) of Cu2O@CBP. The synthesized Cu2O catalysts demonstrated efficient degradation of methylene blue (MB) used as a model as recalcitrant compounds under LED-driven visible light photocatalysis and heterogeneous Fenton-like reactions with hydrogen peroxide (H2O2) using the degradation percentage and the first-order apparent degradation rate constant (kapp). The degradation efficiency of MB was pH-dependent, with neutral pH favoring photocatalysis (kapp = 0.00718 min−1) due to enhanced hydroxyl (·OH) and superoxide radical (O2·−) production, while acidic pH conditions improved Fenton-like reaction efficiency (kapp = 0.00812 min−1) via ·OH. The reusability of the photocatalysts was also evaluated, showing a decline in performance for Fenton-like reactions at acidic pH about 22.76% after five cycles, while for photocatalysis at neutral pH decline about 11.44% after five cycles. This research provides valuable insights into the catalytic mechanisms and supports the potential of eco-friendly Cu2O nanoparticles for sustainable wastewater treatment applications.

Degradation of Methyl Orange from Aqueous Solution Using Fe-Ni-Co-Based Trimetallic Nanocomposites: Optimization by Response Surface Methodology

Effluent-containing dye molecules is a significant environmental hazard. An economical and energy-saving solution is needed to combat this issue for the purpose of environmental sustainability. In this study, Fe-Ni-Co-based trimetallic nanocomposite was synthesized using the coprecipitation method. Scanning Electron Microscopy (SEM), X-ray diffraction (XRD), and Fourier Transform Infra-Red spectroscopy were conducted to explore the physical morphology, phase structure and functional groups of the synthesized catalyst. Among dyes, methyl orange is considered as a major contaminant in textile effluent. The current study focused on the degradation of methyl orange using a trimetallic Fe-Ni-Co-based nanocomposite. A central composite design in response surface methodology was employed to analyze the independent variables including dye concentration, catalyst dose, temperature, hydrogen peroxide, irradiation time, and pH. Dye degradation has been achieved up to 81% in 20 min at the lowest initial concentration (5 mg/L) in optimized conditions. Based on ANOVA, the predicted values were in great agreement with the actual values, signifying the applicability of response surface methodology in the photocatalytic decolorization of dyeing effluents. The results gained from this research demonstrated that the synthesis method of trimetallic nanocomposite (Iron Triad) is a cost-effective and energy efficient method that can be scaled up to a higher level for industrial application.