Search Results (17)

This paper discusses the fabrication of three-dimensional dendritic Ag nanostructures, showcasing pronounced Localized Surface Plasmon Resonance (LSPR) effects. These nanostructures, employed in surface-enhanced Raman scattering (SERS), function as sensors for lactic acid in artificial sweat. The dendritic structures of the silver nanoparticles (AgNPs) create an effective SERS substrate, with additional hotspots at branch junctures enhancing LSPR. We achieve differential LSPR effects by varying the distribution and spacing of branches and the overall morphology. Adjustments to electrodeposition parameters, such as current and plating solution protective agents on an anodized aluminum oxide (AAO) base, allow for precise control over LSPR intensities. By pre-depositing AgNPs, the electron transmission paths during electrodeposition are modified, which leads to optimized dendritic morphology and enhanced LSPR effects. Parameter optimization produces elongated rods with main and secondary branches, covered with uniformly sized, densely packed, non-overlapping spherical AgNPs. This configuration enhances the LSPR effect by generating additional hotspots beyond the branch tips. Fine-tuning the electrodeposition parameters improved the AgNPs’ morphology, achieving uniform particle distribution and optimal spacing. Compared to non-SERS substrates, our structure amplified the Raman signal for lactic acid detection by five orders of magnitude. This method can effectively tailor SERS substrates for specific analytes and laser-based detection. Full article

The purpose of the study was to synthesize and investigate the influence of geometrical structure, magnetism, and cytotoxic activity on core–shell platinum and iron–platinum (Fe/Pt) composite nanowires (NWs) for potential application in targeted chemotherapeutic approaches. The Pt-NWs and Fe/Pt composite NWs were synthesized via template electrodeposition, using anodic aluminum oxide (AAO) membranes. The Fe/Pt composite NWs (Method 1) was synthesized using two electrodeposition steps, allowing for greater control of the diameter of the NW core. The Fe/Pt composite NWs (Method 2) was synthesized by pulsed electrodeposition, using a single electrolytic bath. The properties of the synthesized NWs were assessed by high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, powder X-ray diffraction (XRD), inductively coupled plasma–optical emission spectrometry (ICP-OES), vibrating-sample magnetometry (VSM), and surface charge (zeta potential). A microscopy image analysis of the NWs revealed the presence of high-aspect-ratio NWs with nominal diameters of 40–50 nm and lengths of approximately <4 µm. The obtained powder XRD patterns confirmed the presence of a polycrystalline structure for both Pt NWs and Fe/Pt composite NWs. The potential utility of the synthesized NW nanoplatforms for anticancer activity was investigated using Tera 1 cells and Mouse 3T3 cells. Pt-NWs displayed modest cytotoxic activity against Tera 1 cells, while the Fe/Pt composite NWs (both Methods 1 and 2) demonstrated enhanced cytotoxic activity compared to the Pt-NWs on Tera 1 cells. The Fe/Pt composite NWs (Method 1) displayed ferromagnetic behavior and enhanced cytotoxic activity compared to Pt-NWs on Tera 1 cells, thus providing a sound basis for future magnetically targeted chemotherapeutic applications. Full article

The incessant need for the elimination of pathogenic viruses and multi-drug resistant bacteria has been a critical issue during recent decades, and requires the creation of new antimicrobial materials. Our study describes the production of silver-modified anodic alumina substrates by two methods, and estimation of their bactericidal activity. Aluminum oxide coatings were obtained via an anodization process of low-purity aluminum in an acidic bath for different time periods. The realization of silver infiltration into the pores of the alumina layers was carried out employing two different routes—electrochemical deposition, and in situ thermal reduction. The obtained films were characterized using scanning electron microscopy (SEM). Changes in the surface morphology and thickness of the initial oxide structures after hot water sealing procedure were observed. The presence of silver inside the pores of the alumina layers was also assessed. It was found that silver electrodeposition resulted in greater surface saturation. Large silver accumulations were observed on the thinner anodic films which experienced electroplating for longer time periods. Finally, the antibacterial activity of the modified alumina structures against Gram-negative (Escherichia coli) and Gram-positive (Bacillus cereus) bacteria was evaluated. The results demonstrate that silver deposits acquired by the electrochemical technique improve the bactericidal efficiency of the anodic aluminum oxide (AAO) layers. On the contrary, alumina structures with chemically embedded Ag particles did not show significant antibacterial properties. Overall, the present studies demonstrate that biological activity of silver-doped AAO films depends on the techniques used for their modification. Full article

The fabrication and characterization of superconducting nanowires fabricated by the anodic aluminium oxide (AAO) template technique has been reviewed. This templating method was applied to conventional metallic superconductors, as well as to several high-temperature superconductors (HTSc). For filling the templates with superconducting material, several different techniques have been applied in the literature, including electrodeposition, sol-gel techniques, sputtering, and melting. Here, we discuss the various superconducting materials employed and the results obtained. The arising problems in the fabrication process and the difficulties concerning the separation of the nanowires from the templates are pointed out in detail. Furthermore, we compare HTSc nanowires prepared by AAO templating and electrospinning with each other, and give an outlook to further research directions. Full article

One-dimensional (1D) nanostructures, such as nanotubes, nanopores, nanodots and nanocones, are characterized by better catalytic properties than bulk material due to their large active surface area and small geometrical size. These structures can be produced by several methods of synthesis including the one- and two-step methods. In the one-step method, a crystal modifier is added to the solution in order to limit the horizontal direction of structures growing during electrodeposition. In this work, NH₄Cl was used as a crystal modifier. Another way of production of 1D nanocones is the electrodeposition of metal in porous anodic alumina oxide (AAO) templates, called the two-step method. In this case, the AAO template was obtained using a two-step anodization process. Nanocones obtained by the two-step method show smaller geometrical size. In this work, cobalt nanoconical structures were obtained from an electrolyte containing CoCl₂ and H₃BO₃. The electrocatalytic properties of materials fabricated by one-step and two-step methods were measured in 1 M NaOH and compared with bulk material electrodeposited from the same electrolyte. There were several microshell structures in the case of Co deposits obtained by the one-step method. To solve this problem, different conditions of synthesis Co cones by the one-step method were applied. The electrocatalytic activity of these samples was checked as well. Full article

Porous anodic alumina oxide (AAO) obtained via two-step anodization is a material commonly used as a template for fabricating 1D nanostructures. In this work, copper and cobalt-iron 1D nanocones were obtained by an electrodeposition method using AAO templates. The templates were produced using two-step anodization in H₂C₂O₄. The Co–Fe nanostructures are characterized by homogeneous pore distribution. The electrocatalytic activity of the produced nanomaterials was determined in 1 M NaOH using the linear sweep voltammetry (LSV) and chronopotentiometry (CP) methods. These materials can be used as catalysts in the water-splitting reaction. The sample’s active surface area was calculated and compared with bulk materials. Full article

The electrochemical preparation of arrays of copper ultramicrowires (CuUWs) by using porous membranes as templates is critically revisited, with the goal of obtaining cheap but efficient substrates for surface enhanced Raman spectroscopy (SERS). The role of the materials used for the electrodeposition is examined, comparing membranes of anodized aluminum oxide (AAO) vs. track-etched polycarbonate (PC) as well as copper vs. glassy carbon (GC) as electrode material. A voltammetric study performed on bare electrodes and potentiostatic tests on membrane coated electrodes allowed the optimization of the deposition parameters. The final arrays of CuUWs were obtained by chemical etching of the template, with NaOH for AAO and CH₂Cl₂ for PC. After total etching of the template, SERS spectra were recorded on CuUWs using benzenethiol as SERS probe with known spectral features. The CuUW substrates displayed good SERS properties, providing enhancement factor in the 10³–10⁴ range. Finally, it was demonstrated that higher Raman enhancement can be achieved when CuUWs are decorated with silver nanostars, supporting the formation of SERS active hot-spots at the bimetallic interface. Full article

One-dimensional (1D) nanostructures, such as nanotubes, nanopores, nanodots and nanocones, are characterized by better catalytic properties than bulk materials due to their large active surface area and small geometrical size. There are several methods of synthesis for these structures, including the one- and two-step methods. In the one-step method, a crystal modifier is added to the solution in order to limit the horizontal direction of structures growing during electrodeposition. In this work, cobalt nanoconical structures were obtained from an electrolyte containing CoCl₂, H₃BO₃ and NH₄Cl as the crystal modifier. Another method of production of 1D nanocones is electrodeposition of the metal into porous anodic alumina oxide (AAO) templates. This method is called the two-step method. In this case, an AAO template was obtained using two-step anodization. Then, electrodeposition of cobalt was performed from an electrolyte containing CoSO₄ and H₃BO₃. Nanocones obtained by the two-step method show smaller geometrical size. The bulk sample was electrodeposited from the same electrolyte. The electrocatalytic properties of materials fabricated by the one-step and two-step methods were measured in 1M NaOH and compared with bulk materials. Co cones obtained by the one-step method show the worst electrocatalytic properties. The hydrogen evolution reaction started the earliest for Co nanocones electrodeposited in the templates. Full article

In this study, CuInSe₂ (CIS) films (CIS-TFs) and nanorods (CIS-NRs) were successfully deposited on Mo/glass and p⁺-silicon (p⁺-Si) using an electrodeposition method. Anodic aluminum oxide (AAO) was used as the template when the CIS-NRs were deposited. Pt, indium tin oxide (ITO), and Ag were deposited as the upper electrodes using a sputtering method to form the hetero-junction devices of Pt/CIS-NRs/p⁺-Si, ITO/CIS-NRs/p⁺-Si, ITO/CIS-TF/Mo/glass, and Ag/CIS-NRs/p⁺-Si, respectively. When p⁺-Si was used as the substrate, Al was deposited on p⁺-Si to form negative electrodes for the devices of Pt/CIS-NRs/p⁺-Si, ITO/CIS-NRs/p⁺-Si, and Ag/CIS-NRs/p⁺-Si. The current–voltage properties of all the hetero-junction devices were measured and we found that the hetero-junction of ITO/CIS-NRs/p⁺-Si, ITO/CIS-TF/Mo/glass, and Ag/CIS-NRs/p⁺-Si devices revealed the properties of Schottky diodes but the hetero-junction device of Pt/CIS-NRs/p⁺-Si device did not. The reason for the cause of the differences between these hetero-junction devices was investigated for this study. Full article

Interdiffusion between Si substrate and nanorod arrays of Au, Pt, and AuPt nanoalloys is investigated at temperatures lower than the AuSi eutectic temperature. When the nanorod is pure Au, Si diffusion from the substrate is very rapid. Au atoms are completely replaced by Si, converting the nanostructure into one of Si nanorod arrays. Au is diffused out to the substrate. The Au nanorod arrays on Si are unstable. When the nanorod is pure Pt, however, no diffusion of Si into the nanorod or any silicide formation is observed. The Pt nanorods are stable on Si substrate. When the nanorods are an alloy of AuPt, interesting interactions occur. Si diffusion into the nanorods is rapid but the diffusing Si readily reacts with Pt forming PtSi while Au diffuses out to the substrate. After annealing, nanophases of Au, Pt, PtSi, and Si may be present within the nanorods. When the Pt content of the alloy is low (12 at%) all Pt atoms are converted to silicide and the extra Si atoms remain in elemental form, particularly near the tip of the nanorods. Hence, the presence of Au accelerates Si diffusion and the ensuing reaction to form PtSi, a phenomenon absents in pure Pt nanorods. When the Au content of the alloy is low, the Si diffusion would cease when all Au atoms have diffused out of the nanorod, thereby arresting the silicide formation resulting in excess Pt in elemental form within the nanorod. This is a technique of making Si nanorods with and without embedded PtSi nanophase consisting of heterojunctions which could have unique properties. Full article

The time-dependence of electrochemical reduction current, which was observed during the one-dimensional (1-D) crystal growth of ferromagnetic cobalt nanowire arrays, was analyzed by Johnson–Mehl–Avrami–Kolmogorov (JMAK) theory. Textured hcp-Co nanowire arrays were synthesized by potentio-static electrochemical reduction of Co²⁺ ions in anodized aluminum oxide (AAO) nanochannel films. Crystal growth geometry factor n in the JMAK equation was determined to be ca. 1. Hence, the electrochemical crystal growth process of a numerical nanowires array can be explained by 1-D geometry. The crystal nucleation frequency factor, k in JMAK equation was estimated to be the range between 10⁻⁴ and 10⁻³. Our experimental results revealed that the crystal nucleation site density N_d increased up to 2.7 × 10⁻⁸ nm⁻³ when increasing the overpotential for cobalt electrodeposition by shifting the cathode potential down to −0.85 V vs. Ag/AgCl. The (002) crystal orientation of hcp-Co nanowire arrays was, remarkably, observed by decreasing N_d. Spontaneous magnetization behavior was observed in the axial direction of nanowires. By decreasing the overpotential for cobalt electrodeposition, the coercivity of the nanocomposite film increased and reached up to 1.88 kOe, with a squareness of ca. 0.9 at room temperature. Full article

Hybrid materials play an essential role in the development of the energy storage technologies since a multi-constituent system merges the properties of the individual components. Apart from new features and enhanced performance, such an approach quite often allows the drawbacks of single components to be diminished or reduced entirely. The goal of this paper was to prepare and characterize polymer-metal hydroxide (polypyrrole-nickel hydroxide, PPy-Ni(OH)₂) nanowire arrays demonstrating good electrochemical performance. Nanowires were fabricated by potential pulse electrodeposition of pyrrole and nickel hydroxide into nanoporous anodic alumina oxide (AAO) template. The structural features of as-obtained PPy-Ni(OH)₂ hybrid nanowires were characterized using FE-SEM and TEM analysis. Their chemical composition was confirmed by energy-dispersive x-ray spectroscopy (EDS). The presence of nickel hydroxide in the synthesized PPy-Ni(OH)₂ nanowire array was investigated by X-ray photoelectron spectroscopy (XPS). Both FE-SEM and TEM analyses confirmed that the obtained nanowires were composed of a polymer matrix with nanoparticles dispersed within. EDS and XPS techniques confirmed the presence of PPy-Ni(OH)₂ in the nanowire array obtained. Optimal working potential range (i.e., available potential window), charge propagation, and cyclic stability of the electrodes were determined with cyclic voltammetry (CV) at various scan rates. Interestingly, the electrochemical stability window for the aqueous electrolyte at PPy-Ni(OH)₂ nanowire array electrode was remarkably wider (ca. 2 times) in comparison with the non-modified PPy electrode. The capacitance values, calculated from cyclic voltammetry performed at 20 mV s⁻¹, were 25 F cm⁻² for PPy and 75 F cm⁻² for PPy-Ni(OH)₂ array electrodes. The cyclic stability of the PPy nanowire array electrode up to 100 cycles showed a capacitance fade of about 13%. Full article

Though copper nano-pillars (CNPs) filled in anodic aluminum oxide (AAO) film has been developed for many years, the high pore-filling percentage in AAO is still a bottleneck. We have demonstrated a new electrodeposition method to fill CNPs in AAO without the seed layer which is required in the traditional electrodeposition process. CNPs with uniform heights were obtained and the pore-filling percentage reached up to 97.5%. Low current density is beneficial for the high pore-filling percentage due to the uniform growing rate in different nanoscale pores. The high temperature increased the diffusion velocity of ions and enhanced the pore filling percentage but also corroded the AAO film simultaneously. Results showed that CNPs grains with <220> orientation were fabricated. Electrodeposition with low electric current could contribute to the forming of CNPs with (220) preferred orientation due to the promotion of dehydration reduction processes. The thermal conductivities of Cu-AAO interposers reaches 92.34 W/(m·K) and 3.19 W/(m·K) in vertical and horizontal directions, respectively. Full article

The formation work of a two-dimensional hcp-Co (metallic cobalt crystal with hexagonal close packed structure) nucleus, W_hkl, was calculated by Pangarov’s theory. W₀₀₂ was estimated to be smaller than W₁₀₀ in a cathode potential range nobler than the transition potential, E^tra (ca. −0.77 V vs. Ag/AgCl). To confirm the above estimation, ferromagnetic nanocomposite thick films, which contained (002) textured hcp-Co nanocrystal arrays, were synthesized by potentiostatic electrochemical reduction of Co²⁺ ions in anodized aluminum oxide (AAO) nanochannel films with ca. 45 µm thickness. The aspect ratio of hcp-Co nanocrystals with a diameter of ca. 25 nm reached up to ca. 1800. Our experimental results revealed that the texture coefficient, TC₀₀₂, increased when decreasing the overpotential for hcp-Co electrodeposition by shifting the cathode potential nobler than E^tra. In a similar way, TC₀₀₂ increased sharply by decreasing the growth rate of the hcp-Co nanocrystals so that it was smaller than the transition growth rate, R^tra (ca. 600 nm s⁻¹). The perpendicular magnetization performance was observed in AAO nanocomposite films containing hcp-Co nanocrystal arrays. With increasing TC₀₀₂, the coercivity of the nanocomposite film increased and reached up to 1.66 kOe, with a squareness of ca. 0.9 at room temperature. Full article

Self-standing Bi₂Te₃ networks of interconnected nanowires were fabricated in three-dimensional porous anodic alumina templates (3D–AAO) with a porous structure spreading in all three spatial dimensions. Pulsed electrodeposition parameters were optimized to grow highly oriented Bi₂Te₃ interconnected nanowires with stoichiometric composition inside those 3D–AAO templates. The nanowire networks were analyzed by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX), and Raman spectroscopy. The results are compared to those obtained in films and 1D nanowires grown under similar conditions. The crystalline structure and composition of the 3D Bi–Te nanowire network are finely tuned by controlling the applied voltage and the relaxation time off at zero current density during the deposition. With this fabrication method, and controlling the electrodeposition parameters, stoichiometric Bi₂Te₃ networks of interconnected nanowires have been obtained, with a preferential orientation along [1 1 0], which makes them optimal candidates for out-of-plane thermoelectric applications. Moreover, the templates in which they are grown can be dissolved and the network of interconnected nanowires is self-standing without affecting its composition and orientation properties. Full article