RESUMEN
The unique structural and electrochemical properties of graphene oxide (GO) make it an ideal material for the fabrication of biosensing devices. Therefore, in the present study, graphene oxide nanoparticles modified paper electrodes were used as a low-cost matrix for the development of an amperometric DNA sensor. The graphene oxide was synthesized using the modified hummers method and drop cast on a screen-printed paper electrode (SPPE) to enhance its electrochemical properties. Further, the GO/SPPE electrode was modified with a 5'NH2 labeled ssDNA probe specific to the htrA gene of Orientia tsutsugamushi using carbodiimide cross-linking chemistry. The synthesized GO was characterized using UV-Vis, FTIR, and XRD. The layer-by-layer modification of the paper electrode was monitored via FE-SEM, cyclic voltammetry, and electrochemical impedance spectroscopy (EIS). The sensor response after hybridization with single-stranded genomic DNA (ssGDNA) of O. tsutsugamushi was recorded using differential pulse voltammetry (DPV). Methylene blue (1 mM in PBS buffer, pH 7.2) was used as a hybridization indicator and [Fe(CN)6]-3/-4 (2.5 mM in PBS buffer, pH 7.2) as a redox probe during electrochemical measurements. The developed DNA sensor shows excellent sensitivity (1228.4 µA/cm2/ng) and LOD (20 pg/µL) for detection of O. tsutsugamushi GDNA using differential pulse voltammetry (DPV).
Asunto(s)
Técnicas Biosensibles , Grafito , Nanopartículas , ElectrodosRESUMEN
The modern development of nanotechnology requires the discovery of simple approaches that ensure the controlled formation of functional nanostructures with a predetermined morphology. One of the simplest approaches is the self-assembly of nanostructures. The widespread implementation of self-assembly is limited by the complexity of controlled processes in a large volume where, due to the temperature, ion concentration, and other thermodynamics factors, local changes in diffusion-limited processes may occur, leading to unexpected nanostructure growth. The easiest ways to control the diffusion-limited processes are spatial limitation and localized growth of nanostructures in a porous matrix. In this paper, we propose to apply the method of controlled self-assembly of gold nanostructures in a limited pore volume of a silicon oxide matrix with submicron pore sizes. A detailed study of achieved gold nanostructures' morphology, microstructure, and surface composition at different formation stages is carried out to understand the peculiarities of realized nanostructures. Based on the obtained results, a mechanism for the growth of gold nanostructures in a limited volume, which can be used for the controlled formation of nanostructures with a predetermined geometry and composition, has been proposed. The results observed in the present study can be useful for the design of plasmonic-active surfaces for surface-enhanced Raman spectroscopy-based detection of ultra-low concentration of different chemical or biological analytes, where the size of the localized gold nanostructures is comparable with the spot area of the focused laser beam.
RESUMEN
This work examined the influence of zirconium concentration on barium titanate (BZT) BaZrxTi1-xO3, with (x = 0, 0.15, 0.50, 0.75, and 1), produced by the tartrate precursor technique. The Fourier transform infrared (FTIR) spectra support the X-ray diffraction (XRD) results regarding formation of the perovskite structure. Grain size grows with Zr concentration, suggesting that the presence of Zr ions enlarges the grains. The transmission electron microscopy (TEM) images demonstrated that, due to their nano size, nanocrystallites are agglomerated in most images with irregular morphologies and average particle sizes from 20.75 nm to 63.75 nm. Increasing Zr content diminished the piezoelectric coefficient (d33) and the grain size. The value of d33 decreases by increasing Zr content, and there is an inverse relationship between grain size and d33. The remnant polarization of BZT increases with increasing Zr4+ content, which may be suitable for permanent memory device applications.
RESUMEN
Single crystals of Cu2ZnGeSe4 and Cu2ZnGeS4 solid solutions were developed and successfully obtained using the chemical vapor transfer method, with iodine acting as a transporter. The structure, compositional dependences of lattice parameters, pycnometric and X-ray densities and microhardness were determined. The chemical composition determined by the X-ray microanalysis satisfactorily corresponds to the nominal one with a tolerance of ±5 %. The XRD analysis showed that all the obtained compounds and their solid solutions have unit cell described by tetragonal symmetry. The attice parameters were found to be а = 5.342 ± 0.005 Å, Ñ = 10.51 ± 0.01 Å for the Сu2ZnGeS4 compound and а = 5.607 ± 0.005 Å, Ñ = 11.04 ± 0.01 Å for the Cu2ZnGeSe4, respectively. Structural studies confirmed the validity of the Vegard's law in relation to the obtained samples. The pycnometric densities of â¼4.28 g/cm3 for the Cu2ZnGeS4 and â¼5.46 g/cm3 for the Cu2ZnGeSe4 were found to be slightly less than their X-ray densities of â¼4.32 g/cm3 and â¼5.52 g/cm3, respectively. The maximum microhardness of â¼398 kg/mm2 for these solid solutions corresponds to x = 0.60. The melt point of the solid solutions increases from â¼1180 °C for the Сu2ZnGeSe4 up to â¼1400 °C for the Сu2ZnGeS4. Based on X-ray fluorescence analysis and DTA data, the phase diagram of the Cu2ZnGeSe4-Cu2ZnGeS4 system was constructed. Analysis of the obtained diagram indicates its first type according to Rozbom's classification.
RESUMEN
It is common knowledge that the O2 evolution reaction (OER) is a crucial half-reaction in the electrolysis of water. However, it is currently difficult to create inexpensive OER electrode materials in a way that is efficient, simple, and environmentally friendly. In this research, metal oxy-hydroxides with numerous oxygen defects (M-OOHv) are created at surface of Cu foam (CF) using a unique, straightforward electro-oxidation reconstitution (ER) process. Different spectroscopic and microscopy methods are used to analyse the electrode characteristics of Al2Cu-MOF@M-OOHv-ER/CF; electrochemical measurements display a lower overpotential (η) of 366 mV @ 10 mA cm-2 and a Tafel slope of 95.2 mV dec-1 in 1.0 M KOH. X-Ray diffraction (XRD), scanning electron microscopy (SEM), and Raman studies confirm the phase transition of the metal-organic framework (MOF) to the M-OOH, which acts as the active site to boost the OER activity. Through spectroscopic and microscopic investigations, it is determined that the efficiency of bimetallic electrode materials and oxygen vacancies in the M-OOHv have an impact on the electron power density. The manufactured electrode material additionally showed good durability for 50 hours. As a result, the newly developed Al2Cu-MOF@M-OOHv-ER/CF nanomaterial has greater potential for both electrolysis of water and other energy storage equipment.
RESUMEN
This study announces the anomalous phase separation in CoNiP alloy electroplating. The observed phenomenon of the formation of magnetic bubbles was described for the first time for this triple CoNiP system. This study briefly covers all stages of magnetic bubble formation, starting from the formation of an amorphous phosphor-rich sublayer, followed by nucleation centers, and finally cobalt-rich bubbles. An explanation for the anomalous mechanism of bubble formation was found in the effects of additives and the phenomena of depolarization and superpolarization.
RESUMEN
Structural, electronic, elastic and magnetic properties of CeCu3-x Mn x V4O12 (x = 0, 1, 2 and 3) system have been carried out through DFT using GGA, GGA+U and HF potential. The investigation of structural optimization reveals that lattice parameters of the understudy system is reliable with the reported results and are increasing with the Mn substitution due to their greater atomic radii as compare to Cu atom. Both the cohesive energy and the enthalpy show that CeCu3V4O12 is the most thermodynamically stable among these compounds. When Mn is replaced by Cu in these compounds, not only it become semi-metals, but the host compound also changes from non-magnetic to anti-ferromagnetic and their electrical resistance provides further credence to their electronic behavior. Mechanical stability, anisotropy, and ductility are all demonstrated through the elastic characteristics of these compounds. Due to anti-ferromagnetic ductile nature of the Mn base compounds, it is expected that the compounds in the system may use for spintronic application and in magnetic cloaking devices.
RESUMEN
The polycrystalline SrFe12O19 samples deeply substituted up to at.67% by Al3+, Ga3+, In3+, Co3+, and Cr3+ cations with a high configurational mixing entropy were prepared by solid-phase synthesis. Phase purity and unit cell parameters were obtained from XRD and analyzed versus the average ionic radius of the iron sublattice. The crystallite size varied around â¼4.5 µm. A comprehensive study of the magnetization was realized in various fields and temperatures. The saturation magnetization was calculated using the Law of Approach to Saturation. The accompanying magnetic parameters were determined. The magnetic crystallographic anisotropy coefficient and the anisotropy field were calculated. All investigated magnetization curves turned out to be nonmonotonic. The magnetic ordering and freezing temperatures were extracted from the ZFC and FC curves. The average size of magnetic clusters varied around â¼350 nm. The high values of the configurational mixing entropy and the phenomenon of magnetic dilution were taken into account.
RESUMEN
W-Bi2O3 composites were fabricated using the hot isostatic pressing technique for the first time. The duration of the samples sintering was 3 minutes under conditions of high pressure and temperature. The study of microstructural features and chemical composition of sintered samples was carried out using scanning electron microscopy and energy-dispersive X-ray spectroscopy, respectively. The effect of temperature on the quality of the obtained W-Bi2O3 composites is determined. The densest samples were obtained at a pressure of 5 GPa and temperatures of 25 °C and 500 °C, the densities of which were 18.10 and 17.85 g cm-3, respectively. It is presented that high temperature exposure during sintering adversely affects both the composite density and microstructure due to the redox reaction accompanied by the reduction of Bi and the oxidation of W. The results of the W-Bi2O3 structure study using X-ray diffraction analysis showed that all samples included the main bulk-centered cubic W phase. The presence of the WO2 phase is noted only when the sintering temperature is increased up to 850 °C, which is confirmed by the appearance of diffraction peaks that correspond to 111 and 22-2 crystallographic planes. The shielding efficiency of the W-Bi2O3 composite against gamma radiation using the Phy-X/PSD software was evaluated. A Co60 isotope with an energy of 0.826-2.506 MeV was used as a source of gamma radiation. The calculation results were compared with those for Pb and Bi. Key shielding parameters such as the linear attenuation coefficient, half-value layer, tenth-value layer, mean free path, and effective atomic number are determined. The calculation results revealed that the W-Bi2O3 composite surpasses Pb and Bi in its shielding properties, which makes it promising for use as a prospective material for radiation shielding applications.
RESUMEN
Nanocomposite films based on spinel ferrite (Mg0.8Zn0.2Fe1.5Al0.5O4) in a PVA matrix were obtained. An increase in the spinel concentration to 10 wt.% caused an avalanche-like rise in roughness due to the formation of nanoparticle agglomerates. The lateral mode of atomic force microscopy (AFM) allowed us to trace the agglomeration dynamics. An unexpected result was that the composite with 6 wt.% of filler had a low friction coefficient in comparison with similar composites due to the successfully combined effects of low roughness and surface energy. The friction coefficient decreased to 0.07 when the friction coefficient of pure PVA was 0.72. A specially developed method for measuring nano-objects' surface energy using AFM made it possible to explain the anomalous nature of the change in tribological characteristics.
RESUMEN
Co-Ni ferrite is one of the crucial materials for the electronic industry. A partial substitution with a rare-earth metal brings about modification in crystal lattice and broadens knowledge in the discovery of new magnetic material. Current work reports a Ga3+ substitution in the Co-Ni ferrite with composition Co0.5Ni0.5Fe2-xGaxO4 (where x = 0.0, 0.2, 0.4, 0.6, 0.8, and 1.0), herein referred to as spinel ferrite microspheres (CoNiGa-SFMCs). The samples were crystallized hydrothermally showing a hollow sphere morphology. The crystal phase, magnetic, morphology, and optical behaviour were examined using various microscopy and spectroscopic tools. While the XRD confirmed the phase of SFMCs, the crystallite size varied between 9 and 12 nm. The Tauc plot obtained from DRS (diffuse reflectance spectroscopy) shows the direct optical energy bandgap (Eg) of the products, with the pristine reading having the value of 1.41 eV Eg; the band gap increased almost linearly up to 1.62 eV along with rising the Ga3+ amount. The magnetic features, on the other hand, indicated the decrease in coercivity (Hc) as more Ga3+ is introduced. Moreover, there was a gradual increase in both saturation magnetization (Ms) and magnetic moment (nB) with increasing amount of Ga3+ till x = 0.6 and then a progressive decline with increases in the x content; this was ascribed to the spin-glass-like behavior at low temperatures. It was detected that magnetic properties correlate well with crystallite/particle size, cation distribution, and anisotropy.
RESUMEN
The structural, electrical, and magneto-elastic properties of lanthanide base nitride (Ln = Dy-Lu) anti-perovskites were investigated using density functional theory (DFT). The reported structural outcomes are consistent with the experiment and decrease from Dy to Lu due to the decrease ofatomic radii of Ln atoms. According to the electronic band profile, the metallic characteristics of these compounds are due to the crossing over of Ln-f states at the Fermi level and are also supported by electrical resistivity. The resistivity of these compounds at room temperature demonstrates that they are good conductors. Their mechanical stability, anisotropic, load-bearing, and malleable nature are demonstrated by their elastic properties. Due to their metallic and load-bearing nature, in addition to their ductility, these materials are suitable as active biomaterials, especially when significant acting loads are anticipated, such as those experienced by such heavily loaded implants as hip and knee endo-prostheses, plates, screws, nails, dental implants, etc. In thesecases, appropriate bending fatigue strength is required in structural materials for skeletal reconstruction. Magnetic properties show that all compounds are G-type anti-ferromagnetic, with the Neel temperatures ranging from 24 to 48 K, except Lu3Nin, which is non-magnetic. Due to their anti-ferromagnetic structure, magnetic probes cannot read data contained in anti-ferromagnetic moments, therefore, data will be unchanged by disrupted magnetic field. As a result, these compounds can be the best candidates for magnetic cloaking devices.
RESUMEN
In this study, SrFe12-xNdxO19, where x = 0, 0.1, 0.2, 0.3, 0.4, and 0.5, was prepared using high-energy ball milling. The prepared samples were characterized by X-ray diffraction (XRD). Using the XRD results, a comparative analysis of crystallite sizes of the prepared powders was carried out by different methods (models) such as the Scherrer, Williamson-Hall (W-H), Halder-Wagner (H-W), and size-strain plot (SSP) method. All the studied methods prove that the average nanocrystallite size of the prepared samples increases by increasing the Nd concentration. The H-W and SSP methods are more accurate than the Scherer or W-H methods, suggesting that these methods are more suitable for analyzing the XRD spectra obtained in this study. The specific saturation magnetization (σs), the effective anisotropy constant (Keff), the field of magnetocrystalline anisotropy (Ha), and the field of shape anisotropy (Hd) for SrFe12-xNdxO19 (0 ≤ x ≤ 0.5) powders were calculated. The coercivity (Hc) increases (about 9% at x = 0.4) with an increasing degree of substitution of Fe3+ by Nd3+, which is one of the main parameters for manufacturing permanent magnets.
RESUMEN
The soft/soft (CoFe2O4) x : (Ni0.4Cu0.2Zn0.4Fe2O4) y (CFO x /NCZO y ) nanocomposites (NCs) based on spinel ferrites were produced by the sol-gel method with varying phase's ratio (x : y = 0 : 1; 1 : 1; 2 : 1; 3 : 1; 1 : 3; 1 : 2 and 1 : 0). All NCs consisted of 2 single phases (initial spinels) without any impurities and the absence of chemical interaction between phases. Structural features were investigated and analyzed. The varying of the structural parameters was non-linear and correlated well with the lattice parameter for initial components. There were two maxima observed for all NCs on particle size distribution. It was demonstrated that an increase in the CFO content leads to an increase in the most probable size of the coarse fraction and a decrease in the most probable grain size of the fine fraction. An increase in the NCZO content leads to a decrease in the average size of both fine and coarse fractions. This is obviously due to the large number of defects in the NCZO crystal lattice. The high frequency electromagnetic parameters (real and imaginary parts of the permittivity and permeability, reflection losses) were analyzed in the range of 2-10 GHz. The increase of the energy losses with frequency increase was observed. The nature of the attenuation of the reflected energy associated with the electromagnetic absorption processes due to magnetic losses. Maximal values of the electromagnetic absorption were observed for CFO2/NCZO1 (-18.9 dB). This correlates with the lattice parameters of the composites. The result of the electromagnetic characteristics opens broad perspectives for practical applications such kind of NCs for antenna technology (5G technology) and for electromagnetic absorbing coatings.
RESUMEN
Oxygen and hydrogen generated by water electrolysis may be utilized as a clean chemical fuel with high gravimetric energy density and energy conversion efficiency. The hydrogen fuel will be the alternative to traditional fossil fuels in the future, which are near to exhaustion and cause pollution. In the present study, flowery-shaped In2MnSe4 nanoelectrocatalyst is fabricated by anion exchange reaction directly grown on nickel foam (NF) in 1.0 M KOH medium for oxygen evolution reaction (OER). The physiochemical and electrical characterization techniques are used to investigate the chemical structure, morphology, and electrical properties of the In2MnSe4 material. The electrochemical result indicates that synthesized material exhibits a smaller value of Tafel slope (86 mV/dec), lower overpotential (259 mV), and high stability for 37 h with small deterioration in the current density for a long time. Hence, the fabricated material responds with an extraordinary performance for the OER process and for many other applications in the future.
RESUMEN
The rapid development of industries discharges huge amounts of wastewater that contain surface water. For this reason, we used NiO/polydopamine (NiO/PDA) nanocomposite as an efficient material for the removal of Methyl violet 2B from water. It was synthesized and then characterized by Fourier Transform Infrared (FT-IR) spectroscopy, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray (EDX) analysis, Transmission Electron Microscopy (TEM), and Brunauer-Emmett-Teller (BET). The EDX analysis confirmed the presence of O, Ni, N, and C. The composite has an average particle size of 18 nm. Its surface area is 110.591 m2/g. It was found that the efficiency of dye removal by adsorption on NiO/PDA exceeded that of bare NiO. The adsorption capacity of NiO and NiO/PDA are 126 and 284 mg/g, respectively. The effects of adsorbent dose, dye concentration, and pH on the removal efficiency were examined. The efficiency increased with increasing the adsorbent dose and pH, but dropped from 85 to 73% within 30 min as the initial dye concentration was increased from 0.984 to 4.92 mg/L. Such a drop in the removal efficiency is due to the blocking of the surface-active sites of NiO/PDA, with the high population of dye molecules derived from the continuous increase in dye concentration. The adsorption results of the dye fitted well with the pseudo-second-order kinetics and Langmuir isotherm. The reusability data showed that NiO/PDA was stable across three adsorption-regeneration cycles, thus it can be considered a good recyclable and efficient adsorbent. Because of these results, it can be considered that this method can be applied for the treatment of wastewater.
RESUMEN
Multisubstituted barium ferrites with a magnetoplumbite structure were obtained by the method of solid-phase reactions with ferritization and pre-firing. Three-charged, mainly diamagnetic cations Al3+, Cr3+, Ga3+, and In3+ were chosen as substituents for the Fe3+ iron cations, the proportion of which in solid solutions did not exceed 50%. The values of the configurational mixing entropy were calculated for all the compositions. A slight deviation of the chemical composition of the obtained solid solutions from the nominal value was established by the energy-dispersive X-ray spectroscopy method. The phase purity and values of the unit cell parameters were refined from X-ray scattering data using full-profile analysis in the Rietveld method. A non-monotonic behavior of the unit cell parameters as a function of the B-sub-lattice average ionic radius of the magnetoplumbite structure was found. A minimum unit cell volume of ~667.15 Å3 was found for the composition BaFe6.11Al1.56Cr2.17Ga2.16O19 with a B-sub-lattice average ionic radius of ~7.449 Å. The average crystallite size varied within 5.5-6.5 µm. The temperature and field dependencies of the magnetization have been measured. The values of the saturation magnetization, residual magnetization, hysteresis loop squareness, and coercivity at 50 K and 300 K were extracted from the experimental data. Using the Law of Approach to Saturation, the magnetic crystallographic anisotropy coefficient and anisotropy field were calculated. Multisubstitution leads to a significant decrease in such magnetic parameters as the magnetic ordering temperature and spontaneous magnetization at both temperatures. The maximum magnetic ordering temperature of ~297.7 K was found for the composition BaFe5.84Ga6.19O19 with a B-sub-lattice average ionic radius of ~7.586 Å in a field of 500 Oe. A maximum saturation magnetization of ~24.7 emu/g was found for the composition BaFe5.84Ga6.19O19 with a B-sub-lattice average ionic radius of ~7.586 Å at 50 K. A maximum hysteresis loop squareness of ~0.72 was found for the composition BaFe6.11Al1.56Cr2.17Ga2.16O19 with an average ionic radius of ~7.449 Å at 50 K. A maximum magnetic crystallographic anisotropy coefficient of ~2.09 × 105 Erg/g was found for the composition BaFe6.19Al1.25Cr1.57Ga1.74In1.26O19 with a B-sub-lattice average ionic radius of ~7.706 Å at 50 K. The frustrated magnetic state including the nano-sized clusters with an average diameter in the range of 50-200 nm was established from the results of measuring the ZFC and FC temperature magnetizations. The interpretation of the obtained experimental data is carried out taking into account the increased stability of high-entropy phases and regular changes in the intensity of the Fe3+(Al3+, Cr3+, Ga3+, In3+)-O2--Fe3+(Al3+, Cr3+, Ga3+, In3+) indirect superexchange interactions as a result of magnetic dilution of the iron sub-lattice in the magnetoplumbite structure.
RESUMEN
Thin films of beryllium and gold that are several tens of nanometers thick were obtained, for the first time, on silicon and quartz substrates by the ion-beam method with tenfold alternation of deposition and partial sputtering of the nanosized metal layer. Scanning electron and atomic force microscopy indicate the predominant lateral growth of nanosized metal layers along the substrate surface. Optical spectra indicate the suppression of the localized plasmon resonance. The growth of the film occurs under the influence of the high-energy component of the sputtered metal atoms' flux. The main role in the formation of the nanosized metal film is played by the processes of the elastic collision of incident metal atoms with the atoms of a substrate and a growing metal film. Metal films that are obtained by the tenfold application of the deposition-sputtering of a nanoscale metal layer are characterized by stronger adhesion to the substrate and have better morphological, electrical, and optical characteristics than those that are obtained by means of direct single deposition.
RESUMEN
Binary and ternary composites (CM) based on M-type hexaferrite (HF), polymer matrix (PVDF) and carbon nanomaterials (quasi-one-dimensional carbon nanotubes-CNT and quasi-two-dimensional carbon nanoflakes-CNF) were prepared and investigated for establishing the impact of the different nanosized carbon on magnetic and electrodynamic properties. The ratio between HF and PVDF in HF + PVDF composite was fixed (85 wt% HF and 15 wt% PVDF). The concentration of CNT and CNF in CM was fixed (5 wt% from total HF + PVDF weight). The phase composition and microstructural features were investigated using XRD and SEM, respectively. It was observed that CM contains single-phase HF, γ- and ß-PVDF and carbon nanomaterials. Thus, we produced composites that consist of mixed different phases (organic insulator matrix-PDVF; functional magnetic fillers-HF and highly electroconductive additives-CNT/CNF) in the required ratio. VSM data demonstrate that the main contribution in main magnetic characteristics belongs to magnetic fillers (HF). The principal difference in magnetic and electrodynamic properties was shown for CNT- and CNF-based composites. That confirms that the shape of nanosized carbon nanomaterials impact on physical properties of the ternary composited-based magnetic fillers in polymer dielectric matrix.
RESUMEN
As a contribution to the graphene-based nanoferrite composites, this article is intended to present Mn, Co, and Co-Mn nanoferrites for the preparation and investigation of such samples. Nanoparticles of Co ferrite, Mn ferrite, and Co-Mn ferrite were chemically synthesized by the coprecipitation method. The composites of ferrite/graphene were made by incorporating weight ratios of 25% graphene to 75% ferrite. Various structural and characterizing investigations of ferrite samples and ferrite/graphene composites were performed, including XRD, EDX, SEM, VSM hysteresis loops, AC conductivity, and dielectric behavior. The investigations ensured the formation of the intended nanoferrite powders, each having a single-phase crystal structure with no undesired phases or elements. All samples exhibit a soft magnetic behavior. They show a semiconducting behavior of AC electrical conductivity as well. This was proved by the temperature dependence of the AC's electrical conductivity. Whereas the dielectric function and loss tangent show an expected, well-explained behavior, the ferrite/graphene composite samples have lower saturation magnetization values, lower AC conductivity, and dielectric constant values than the pure ferrites but still have the same behavior trends as those of the pure ferrites. The values obtained may represent steps on developing new materials for expected applications, such as manufacturing supercapacitors and/or improved battery electrodes.