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XPS spectra. High-resolution XPS spectra of (a) Zn 2p, (b) O 1s, and (c) Cu 2p in micro-cross structures of Zn0.67Cu0.33O.
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We report a simple catalyst-free vapor-phase method to fabricate Zn1-xCuxO micro-cross structures. Through a series of controlled experiments by changing the location of the substrate and reaction time, we have realized the continuous evolution of product morphology from nanorods into brush-like structures and micro-cross structures at different po...
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Citations
... Fig. 3(b) shows the Zn 2p XPS spectra. Two peaks at binding energies of 1045.5 and 1022.5 eV were attributable to Zn 2p 1/2 and Zn 2p 3/2 , respectively, indicating the Zn(II) oxidation state [59]. Fig. 3(c) shows the Co 2p XPS spectra. ...
A novel metal coordination-assisted sol-gel method is developed for the synthesis of nanostructures with different architectures, such as nanoparticle-and nanowire-based aerogels. The synergistic effect of composition-derived properties (Co-S or Zn-CoS) and structure-derived properties (zero-dimensional or one-dimensional) on the energy storage capacity was explored by controlling the molar ratio of Zn/Co and architecture of the nanostructures. The one-dimensional Zn-CoS aerogel (Zn/Co = 0.4) exhibited a high specific capacitance (820.2 F g − 1 at 1 A g − 1), high-rate capability (61.1%), and outstanding cyclic stability (96%) after 10,000 cycles. When applied in an asymmetric supercapacitor device, it demonstrated an outstanding energy density of 47.4 W h kg − 1 at a power density of 685.7 W kg − 1 and ultrahigh cyclic performance of 93.8% after 10,000 cycles. Compared with the conventional zero-dimensional aerogel, the nanowire-based aerogel structure offers a shorter pathway for electrons and ions, with similar zinc ion content, resulting in a higher electrical conductivity. Consequently, it effectively demonstrates excellent electrochemical performance as a supercapacitor. The proposed strategy can promote research on the dimensional control of aerogel systems and facilitate the design of other ternary transition-metal-sulfide-based aerogels for use in modern energy devices.
... These losses are crucial for the stability of the film, but at temperatures as high as 700 • C, residual NO x seems to still be retained in the film. The peak appearing at 750 cm −1 corresponds to the vibrational mode of O-La-O [41,42]. ...
... are crucial for the stability of the film, but at temperatures as high as 700 °C, residual NOx seems to still be retained in the film. The peak appearing at 750 cm −1 corresponds to the vibrational mode of O-La-O [41,42]. ...
This article presents the sol-gel method for depositing La2O3 thin films on n-type Si substrates and quartz substrates, and investigates the impact of annealing temperature on the microcomposition, surface morphology, optical properties, and band characteristics of the films. X-ray diffraction (XRD) analysis indicates that the films are amorphous below 500 °C, with annealing resulting in a hexagonal-phase La2O3 (h-a2O3) and new non-hydrated impurities. Fourier-transform infrared (FTIR) analysis reveals that the prepared La2O3 film is unaffected by moisture. Atomic force microscopy (AFM) and scanning electron microscopy (SEM) provide evidence that the La2O3 film has a smooth, uniform surface without cracks. The roughness increases from 0.426 nm to 1.200 nm, and the film thins from 54.85 nm to 49.80 nm as the annealing temperature rises. The film’s transmittance is above 75%, as measured by UV-Vis, and the calculated optical bandgap increases from 5.11 eV to 5.75 eV. The calculated band offset of the La2O3 film is greater than 1 eV, which meets the minimum requirements for MOS devices, thus providing promising prospects for La2O3 films in MOS applications.
... The broad peak centered at 169.0 eV is attributed to the Er 4d spin orbit; Figure 4b [12,103]. In the same way, the peak at 531.5 eV is associated with the oxygen lattice, i.e., O 1s; Figure 4d [7,104]. Moreover, peaks of nickel appeared in the range of 850 eV to 880.0 eV; Figure 4c. ...
Generally, our ecosystem is continuously contaminated as a result of anthropogenic activities that form the basis of our comfort in our routine life. Thus, most scientists are engaged in the development of new technologies that can be used in environmental remediation. Herein, highly calcined binary metal oxide (Er2O3@NiO) semiconductor nanocomposite (NC) was synthesized using a classical wet chemical process with the intention to both detect and degrade the toxic chemicals in an aqueous medium using a novel electrochemical current–potential (I–V) approach for the first time. Optical, morphological, and structural properties of the newly synthesized semiconductor NC were also studied in detail using FT-IR, UV/Vis., FESEM-EDS, XPS, BET, EIS, and XRD techniques. Then, a modified glassy carbon electrode (GCE) based on the newly synthesized semiconductor nanocomposite (Er2O3@NiO-NC/Nafion/GCE) as a selective electrochemical sensor was fabricated with the help of 5% ethanolic-Nafion as the conducting polymer binder in order to both detect and electro-hydrolyze toxic chemicals in an aqueous medium. Comparative study showed that this newly developed Er2O3@NiO-NC/Nafion/GCE was found to be very selective against m-tolyl hydrazine (m-Tolyl HDZN) and to have good affinity in the presence of other interfering toxic chemicals. Analytical parameters were also studied in this approach to optimize the newly designed Er2O3@NiO-NC/Nafion/GCE as an efficient and selective m-Tolyl HDZN sensor. Its limit of detection (LOD) at an SNR of 3 was calculated as 0.066 pM over the linear dynamic range (LDR) of our target analyte concentration (0.1 pM–0.1 mM). The limit of quantification (LOQ) and sensitivity were also calculated as 0.22 pM and 14.50 µAµM−1cm−2, respectively. m-Tolyl HDZN is among the toxic chemicals in our ecosystem that have lethal effects in living beings. Therefore, this newly designed electrochemical sensor based on semiconductor nanostructure material offers, for the first time, a cost-effective technique, in addition to long-term stability, that can be used as an alternative for efficiently probing other toxic chemicals in real samples.
... As shown in Figure 12B, after Zn 2+ adsorption, it was confirmed that the new peaks at approximately 1021.8 and 1045.3 eV in the high-resolution were assigned to Zn2p3/2 and Zn2p1/2, respectively. Moreover, the peak of Na1s at approximately 1073.2 eV significantly decreased to the lowest level, indicating that Zn 2+ was successfully adsorbed onto the surface of the adsorbent via ion exchange [85]. Meanwhile, the appearance of a peak at approximately 124.35 eV indicates that Zn 2+ can further directly react in a few places As shown in Figure 12B, after Zn 2+ adsorption, it was confirmed that the new peaks at approximately 1021.8 and 1045.3 eV in the high-resolution were assigned to Zn2p 3/2 and Zn2p 1/2 , respectively. ...
... Meanwhile, the appearance of a peak at approximately 124.35 eV indicates that Zn 2+ can further directly react in a few places As shown in Figure 12B, after Zn 2+ adsorption, it was confirmed that the new peaks at approximately 1021.8 and 1045.3 eV in the high-resolution were assigned to Zn2p 3/2 and Zn2p 1/2 , respectively. Moreover, the peak of Na1s at approximately 1073.2 eV significantly decreased to the lowest level, indicating that Zn 2+ was successfully adsorbed onto the surface of the adsorbent via ion exchange [85]. Meanwhile, the appearance of a peak at approximately 124.35 eV indicates that Zn 2+ can further directly react in a few places available with OH − resulting in the formation of precipitation compounds (Zn(OH) 2 ) on the surface of synthesized zeolite. ...
... Additionally, the two shakeup satellites are easily observed in the samples at approximately 943.2 and 963.8 eV, which are at a higher binding energy of approximately 7.2 and 9.6 eV above the main Cu2p 3/2 , and at about 9.1 eV above the Cu2p 1/2 peaks, respectively. The presence of strong satellite characteristics of Cu2p excludes the possibility of a Cu 2 O phase [85]. Meanwhile, there was no difference in the peak intensity of Na1s before and after the adsorption experiments, proposing that the Cu 2+ ions were attached to the surface of the adsorbent by surface precipitation or complexation adsorption mechanisms [8], which aligns with the SEM-EDX results in Figure 11a. ...
The increase of global environmental restrictions concerning solid and liquid industrial waste, in addition to the problem of climate change, which leads to a shortage of clean water resources, has raised interest in developing alternative and eco-friendly technologies for recycling and reducing the amount of these wastes. This study aims to utilize Sulfuric acid solid residue (SASR), which is produced as a useless waste in the multi-processing of Egyptian boiler ash. A modified mixture of SASR and kaolin was used as the basic component for synthesizing cost-effective zeolite using the alkaline fusion-hydrothermal method for the removal of heavy metal ions from industrial wastewater. The factors affecting the synthesis of zeolite, including the fusion temperature and SASR: kaolin mixing ratios, were investigated. The synthesized zeolite was characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), particle size analysis (PSD) and N2 adsorption-desorption. The SASR: kaolin weight ratio of 1:1.5 yields faujasite and sodalite zeolite with 85.21% crystallinity, which then shows the best composition and characteristics of the synthesized zeolite. The factors affecting the adsorption of Zn2+, Pb2+, Cu2+, and Cd2+ ions from wastewater on synthesized zeolite surfaces, including the effect of pH, adsorbent dosage, contact time, initial concentration, and temperature, have been investigated. The obtained results indicate that a pseudo-second-order kinetic model and Langmuir isotherm model describe the adsorption process. The maximum adsorption capacities of Zn2+, Pb2+, Cu2+, and Cd2+ ions onto zeolite at 20 °C were 12.025, 15.96, 12.247, and 16.17 mg·g−1, respectively. The main mechanisms controlling the removal of these metal ions from aqueous solution by synthesized zeolite were proposed to be either surface adsorption, precipitation, or ion exchange. The quality of the wastewater sample obtained from the Egyptian General Petroleum Corporation (Eastern Desert, Egypt) was highly improved using the synthesized zeolite and the content of heavy metal ions was significantly reduced, which enhances the utilization of the treated water in agriculture.
... eV and at ~1044.85 eV) suggests a metallic state of the zinc in the coating [68,69]. After the leaching process these bands tends to shift towards lower energies, see Fig. 8(f), probably due to the formation of ZnO, as was suggested by other works [68,70]. ...
... On the other hand, one pair of bands for Zn was found: 1022.00 and 1045.47. The bands can be assigned to zinc oxide (Biesinger et al., 2010;Xu et al., 2013). The next step in identifying the deposit was to carry out X-ray diffraction (XRD) measurements. ...
The endophytic Basidiomycete Sporobolomyces ruberrimus protects its host Arabidopsis arenosa against metal toxicity. Plants inoculated with the fungus yielded more biomass and exhibited significantly fewer stress symptoms in medium mimicking mine dump conditions (medium supplemented with excess of Fe, Zn and Cd). Aside from fine-tuning plant metal homeostasis, the fungus was capable of precipitating Fe in the medium, most likely limiting host exposure to metal toxicity. The precipitated residue was identified by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), X-Ray Diffraction (XRD) and electron microscopy (SEM/TEM) with energy dispersive X-Ray analysis (EDX/SAED) techniques. The performed analyses revealed that the fungus transforms iron into amorphous (oxy)hydroxides and phosphates and immobilizes them in the form of a precipitate changing Fe behaviour in the MSR medium. Moreover, the complexation of free Fe ions by fungi could be obtained by biomolecules such as lipids, proteins, or biosynthesized redox-active molecules.
... As displayed in Figure 5f, the Zn2p orbital exhibits two-spin orbitals Zn2p5/2 and Zn2p3/2, positioned at 1022 and 1045 eV, respectively. The 23.0 eV energy difference between these two spin orbitals confirmed the existence of the Zn 2+ oxidation state in the prepared NCs [33,34]. ...
In this study, a selective 4-nitrophenol (4-NP) sensor was developed onto a glassy carbon electrode (GCE) as an electron-sensing substrate, which decorated with sol–gel, prepared Pt nanoparticles- (NPs) embedded polypyrole-carbon black (PPy-CB)/ZnO nanocomposites (NCs) using differential pulse voltammetry. Characterizations of the NCs were performed using Field Emission Scanning Electron Microscopy (FESEM), Energy-Dispersive Spectroscopy (EDS), X-ray Photoelectron Spectroscopy (XPS), Ultraviolet–visible Spectroscopy (UV–vis), Fourier Transform Infrared Spectroscopy (FTIR), High Resolution Transmission Electron Microscopy (HRTEM), and X-ray Diffraction Analysis (XRD). The GCE modified by conducting coating binders [poly(3,4-ethylenedioxythiophene) polystyrene sulfonate; PEDOT:PSS] based on Pt NPs/PPy-CB/ZnO NCs functioned as the working electrode and showed selectivity toward 4-NP in a phosphate buffer medium at pH 7.0. Our analysis of 4-NP showed the linearity from 1.5 to 40.5 µM, which was identified as the linear detection range (LDR). A current versus concentration plot was formed and showed a regression co-efficient R2 of 0.9917, which can be expressed by ip(µA) = 0.2493C(µM) + 15.694. The 4-NP sensor sensitivity was calculated using the slope of the LDR, considering the surface area of the GCE (0.0316 cm2). The sensitivity was calculated as 7.8892 µAµM−1cm−2. The LOD (limit of detection) of the 4-NP was calculated as 1.25 ± 0.06 µM, which was calculated from 3xSD/σ (SD: Standard deviation of blank response; σ: Slope of the calibration curve). Limit of quantification (LOQ) is also calculated as 3.79 µM from LOQ = 10xLOD/3.3. Sensor parameters such as reproducibility, response time, and analyzing stability were outstanding. Therefore, this novel approach can be broadly used to safely fabricate selective 4-NP sensors based on nanoparticle-decorated nanocomposite materials in environmental measurement.
... Zr3d spectrum (Fig. 3B) reveals the signals at 182.28 and 188.68 eV which are assigned to Zr3d5/2 and Zr3d3/2, respectively [19]. Furthermore, Zn2p spectrum (Fig. 3C) shows the signals at 1022.07 and 1045.13 which are attributed to Zn2p3/2 and Zn2p1/2, respectively [48]. C1s spectrum (Fig. 3D) clarifies the peaks of the carbon-containing groups in the matrix of UiO-66/ZIF-8/PDA@CA at 284.54, 286.75 and 288.92 eV which are assigned to CAC/CAH, CAO/CAN and O@CAO/O@C, respectively [49,50]. ...
Removal of pharmaceutical wastes, especially antibiotics, from aquatic systems is an imperative issue from both human-health and ecological perspectives. Herein, zwitterionic Universitetet i Oslo/Zeolitic imidazolate binary metal-organic framework/[email protected] acetate composite (UiO-66/ZIF-8/[email protected]) were fabricated in the form of floated beads for the adsorptive removal of tetracycline (TC). The formulated composite beads were characterized by FTIR, XRD, SEM, BET, Zeta potential and XPS analysis tools. The results clarified that the composite beads demonstrated positively charged surface at pH < 6.8. Under optimum adsorption conditions, the UiO-66/ZIF-8/[email protected] composite beads demonstrated large specific surface area, good adsorption performance with a relatively short equilibrium time (60 min) and ease separation. Furthermore, the adsorption data fit Temkin > Langmuir > Freundlich with a maximal adsorption capacity of 290.69 mg/g at 25 ◦C, while the adsorption kinetics were well-described by pseudo-second order kinetics. The thermodynamics studies refereed that the adsorption process was endothermic and spontaneous. Besides, the floated UiO-66/ZIF-8/[email protected] beads displayed better adsorption property for eight reuse cycles with a maximal removal (%) reached 67%, reflecting its promising applicability as reusable adsorbent for efficient removal of antibiotics traces from water bodies.
... Variation of the real Z ′ (a) and imaginary Z ′′ (b) parts as function of AC frequency for undoped and Cu-doped ZnO thin films. are attributed to the Wurtzite ZnO structure [29][30][31]. Whereas, the modes A g and B g are assigned to the CuO compound [32,33]. The Raman spectra revealed that the peak position of the two polar modes E 2 high and A 1 (LO) of the Cu-doped ZnO samples coincide with that of undoped ZnO, which is reasonable considering the small mass difference between Cu and Zn, indicating that the Cu-doped ZnO conserves the ZnO hexagonal structure [34]. ...
... engendered by a decrease as well as a broadening of the E 2 high mode (438 cm − 1 ) characteristic of the vibration of the sub-network of oxygen atoms in the Wurtzite ZnO structure, manifested by the attenuation of the (0 0 2) peak as discussed in the XRD results. Otherwise, the intensity of the appeared A g and B g peaks is notably enriched by increasing the copper amount [31][32][33][34][35]. It is important to notice the absence of any vibration modes that may be attributed to the Cu 2 O phase in all the samples [36,37]. ...
... In order to investigate more the valance state of the constituent elements, we show in Fig. 13 the high-resolution XPS spectra of the O 1 s, Zn 2p and Cu 2p peaks contribution before and after the UHV treatment. The high-resolution O 1 s core level peaks shown in Fig. 13.a are broad and asymmetric indicating the involvement of multiple oxygen components (O-Metal at 530.4 eV, O-defects at 531.8 eV and O-Organics at 532.8 eV) [31,[89][90]. The cleaning process reduces the contamination and reshapes the O 1 s core level peaks that become symmetric and well resolved, see Fig. 13.b. ...
In recent years, the contaminated rejects due to the rise of textile and dye industry have dramatically affected the ecosystem and aquatic reserves. In addition, the decontamination of organic species based on nanoparticles as photocatalyst is considered as a complicated route and material consumer. To address the separation issue, it is necessary to develop new methods to degrade organic dyes through coast effective processes. In this context, we present in our study a new photocatalysis design by implementation of the photocatalyst on the inner side surface of transparent glass tube as one piece-photoreactor. Among various Photocatalysis based on metal-oxide materials, zinc oxide is widely studied by tailoring its physical and chemical properties to improve the photocatalytic degradation activity. Accordingly, pure and Cu-doped ZnO catalysts with variable copper amount (1, 2.5 and 4 wt%) were synthesized by ultrasonic spray pyrolysis and characterized by X-ray diffraction (XRD), Raman spectroscopy, UV–visible spectroscopy, Photoluminescence spectroscopy (RT-PL), Atomic force microscopy (AFM), Scanning electron microscopy (SEM), Complex impedance spectroscopy and X-ray photoelectron spectroscopy (XPS). The methylene blue degradation rate was investigated through the decrease of the absorption band situated at 663nm under UV-Vis irradiation. The reusability of the undoped and Cu-doped ZnO photocatalyst tests after six recycles give a steady photodegradation efficiency results
... Figure 1 represents the XPS analysis report of PbO-doped ZnO MSs consisting of O1s, Zn2p, and Pb4f orbitals of existing elements only. As shown in Figure 1a, the Zn2p orbital is split in two spin-orbitals such as Zn2p 3/2 and Zn2p 1/2 located at 1022 and 1045 eV detached with 23.0 eV, which is characteristic value for 2+ ionization state of Zn 2+ in PbO-doped ZnO MSs [40,41]. The O1s orbital as revealed in Figure 1b presents a peak located at 531 eV indicating O 2− ion associated with the Zn-O bond in the PbO-doped ZnO MSs [42,43]. ...
In this approach, a reliable 2,6-dinitrophenol (2,6-DNP) sensor probe was developed by applying differential pulse voltammetry (DPV) using a glassy carbon electrode (GCE) decorated with a wet-chemically prepared PbO-doped ZnO microstructures’ (MSs) electro-catalyst. The nanomaterial characterizing tools such as FESEM, XPS, XRD, UV-vis., and FTIR were used for the synthesized PbO-doped ZnO MSs to evaluate in detail of their optical, structural, morphological, functional, and elemental properties. The peak currents obtained in DPV analysis of 2,6-DNP using PbO-doped ZnO MSs/GCE were plotted against the applied potential to result the calibration of 2,6-DNP sensor expressed by ip(µA) = 1.0171C(µM) + 22.312 (R2 = 0.9951; regression co-efficient). The sensitivity of the proposed 2,6-DNP sensor probe obtained from the slope of the calibration curve as well as dynamic range for 2,6-DNP detection were found as 32.1867 µAµM−1cm−2 and 3.23~16.67 µM, respectively. Besides this, the lower limit of 2,6-DNP detection was calculated by using signal/noise (S/N = 3) ratio and found as good lowest limit (2.95 ± 0.15 µM). As known from the perspective of environment and healthcare sectors, the existence of phenol and their derivatives are significantly carcinogenic and harmful which released from various industrial sources. Therefore, it is urgently required to detect by electrochemical method with doped nanostructure materials. The reproducibility as well as stability of the working electrode duration, response-time, and the analysis of real environmental-samples by applying the recovery method were measured, and found outstanding results in this investigation. A new electrochemical research approach is familiarized to the development of chemical sensor probe by using nanostructured materials as an electron sensing substrate for the environmental safety (ecological system).
