Nanostructured network-like MnO2-NiO composite electrodes were electrodeposited onto stainless steel substrates via different electrodeposition modes, such as chronopotentiometry, chronoamperometry, and cyclic voltammetry, and then subjected to heat treatment at 300°C for metal oxide conversion. X-ray diffraction, field emission scanning electron microscopy, and transmission electron microscopy were used to study the crystalline natures and morphologies of the deposited films. The electrochemical properties were investigated using cyclic voltammetry and charge/discharge tests. The results revealed that the electrochemical performance of the as-obtained composite electrodes depended on the electrodeposition mode. The electrochemical properties of MnO2-NiO composite electrodes prepared using cyclic voltammetry exhibited the highest capacitance values and were most influenced by the deposition cycle number. The optimum specific capacitance was 3509 Fg-1 with energy and power densities of 1322 Wh kg-1 and 110.5 kW kg-1, respectively, at a current density of 20 Ag-1 in a mixed KOH/K3Fe(CN)6 electrolyte.
This study investigates the preliminary efficacy of drug encapsulation in chitosan hydrogels by cathodic electrodeposition for the encapsulation of the aromatic dye methyl orange to enhance drug delivery in biological systems. Chitosan, a biocompatible and transparent polymer, is known for its ability to effectively encapsulate and transport therapeutic agents, which is critical for sustained and targeted drug release. Methyl orange was selected as a model drug to study the effects of deposition and immersion times on encapsulation efficiency. The effects of deposition and immersion times on encapsulation efficiency were analyzed by synthesizing multilayer hydrogels via electrochemical oxidation. Characterization techniques, including UV-visible spectroscopy, FTIR, and NMR, were employed; FTIR indicated an effective absorption of 4.34 % for Td50Ti60, while UV-Vis showed 46.41 % at Td60Ti50. NMR analysis revealed effective concentrations of 0.47 mM for Td70Ti60 and 0.38 mM for Td60Ti50, indicating that longer immersion times enhance absorption. These findings provide a foundation for further studies aimed at optimizing drug delivery strategies and improving the therapeutic efficacy of encapsulated agents in biological applications.
This investigation aims at the reclamation of Cr(VI) from synthetic electroplating industrial effluent by electroextraction process namely electrochemical ion exchange (EIX). An electrochemical ion exchange reactor of desired dimensions was fabricated with the help of ion-permeable membranes, stainless steel cathode and PbO₂ coated Ti expanded mesh anode. The performance of the reactor was studied in batch recirculation mode, continuous flow mode at different experimental conditions. The influence of various experimental factors, for instance, initial metal ion concentration (20, 300, 1000 mg/L of Cr(VI)), applied voltages (2.5 V, 5 V, 7.5 V, 10 V) and flow rates of the process stream (2, 4, 6, 8, 10, 12 and 14 ml/min) on removal/reclamation efficiency was deliberated. For comparison purposes, an electrodialysis process was conducted at the same optimal conditions. It was found that the EIX process with three compartments has more removal efficiency at optimum experimental conditions than the electrodialysis process. The continuous flow process of the reactor with 300 mg/L of Cr(VI) as inlet concentration has studied to predict the breakeven point of the reactor. It was noted that Cr(VI) ion concentration in the treated wastewater is almost zero up to the discharge of 20 liters of treated rinse water.
Mesoporous Mn1.5Co1.5O₄ (MCO) spinel films were prepared directly on a conductive nickel (Ni) foam substrate via electrodeposition and an annealing treatment as supercapacitor electrodes. The electrodeposition time markedly influenced the surface morphological, textural, and supercapacitive properties of MCO/Ni electrodes. The (MCO/Ni)-15 min electrode (electrodeposition time: 15 min) exhibited the highest capacitance among three electrodes (electrodeposition times of 7.5, 15, and 30 min, respectively). Further, an asymmetric supercapacitor that utilizes (MCO/Ni)-15 min as a positive electrode, a plasma-treated activated carbon (PAC)/Ni electrode as a negative electrode, and carboxymethyl cellulose-lithium nitrate (LiNO₃) gel electrolyte (denoted as (PAC/Ni)//(MCO/Ni)-15 min) was fabricated. In a stable operation window of 2.0 V, the device exhibited an energy density of 27.6 Wh·kg-1 and a power density of 1.01 kW·kg-1 at 1 A·g-1. After 5000 cycles, the specific energy density retention and power density retention were 96% and 92%, respectively, demonstrating exceptional cycling stability. The good supercapacitive performance and excellent stability of the (PAC/Ni)//(MCO/Ni)-15 min device can be ascribed to the hierarchical structure and high surface area of the (MCO/Ni)-15 min electrode, which facilitate lithium ion intercalation and deintercalation at the electrode/electrolyte interface and mitigate volume change during long-term charge/discharge cycling.
Efficient solar driven photoelectrochemical (PEC) response by enhancing charge separation has attracted great interest in the hydrogen generation application. The formation of one-dimensional ZnO nanorod structure without bundling is essential for high efficiency in PEC response. In this present research work, ZnO nanorod with an average 500 nm in length and average diameter of about 75 nm was successfully formed via electrodeposition method in 0.05 mM ZnCl₂ and 0.1 M KCl electrolyte at 1 V for 60 min under 70 °C condition. Continuous efforts have been exerted to further improve the solar driven PEC response by incorporating an optimum content of TiO₂ into ZnO nanorod using dip-coating technique. It was found that 0.25 at % of TiO₂ loaded on ZnO nanorod film demonstrated a maximum photocurrent density of 19.78 mA/cm² (with V vs. Ag/AgCl) under UV illumination and 14.75 mA/cm² (with V vs. Ag/AgCl) under solar illumination with photoconversion efficiency ~2.9% (UV illumination) and ~4.3% (solar illumination). This performance was approximately 3-4 times higher than ZnO film itself. An enhancement of photocurrent density and photoconversion efficiency occurred due to the sufficient Ti element within TiO₂-ZnO nanorod film, which acted as an effective mediator to trap the photo-induced electrons and minimize the recombination of charge carriers. Besides, phenomenon of charge-separation effect at type-II band alignment of Zn and Ti could further enhance the charge carrier transportation during illumination.
Miniaturization of electronic devices has led to the development of 3D IC packages which require ultra-small-scale interconnections. Such small interconnects can be completely converted into Cu-Sn based intermetallic compounds (IMCs) after reflow. In an effort to improve IMC based interconnects, an attempt is made to add Ni to Cu-Sn-based IMCs. Multilayer interconnects consisting of stacks of Cu/Sn/Cu/Sn/Cu or Cu/Ni/Sn/Ni/Sn/Cu/Ni/Sn/Ni/Cu with Ni = 35 nm, 70 nm, and 150 nm were electrodeposited sequentially using copper pyrophosphate, tin methanesulfonic, and nickel Watts baths, respectively. These multilayer interconnects were investigated under room temperature aging conditions and for solid-liquid reactions, where the samples were subjected to 250 °C reflow for 60 s and also 300 °C for 3600 s. The progress of the reaction in the multilayers was monitored by using X-ray Diffraction, Scanning Electron Microscope, and Energy dispersive X-ray Spectroscopy. FIB-milled samples were also prepared for investigation under room temperature aging conditions. Results show that by inserting a 70 nanometres thick Ni layer between copper and tin, premature reaction between Cu and Sn at room temperature can be avoided. During short reflow, the addition of Ni suppresses formation of Cu₃Sn IMC. With increasing Ni thickness, Cu consumption is decreased and Ni starts acting as a barrier layer. On the other hand, during long reflow, two types of IMC were found in the Cu/Ni/Sn samples which are the (Cu,Ni)₆Sn₅ and (Cu,Ni)₃Sn, respectively. Details of the reaction sequence and mechanisms are discussed.
A waste material known as palm oil empty fruit bunch (EFB) is used as a source of cellulose for the development of polymeric materials for the removal of metal ions from industrial wastewater. A poly(acrylonitrile)-grafted palm cellulose copolymer was synthesized by a conventional free radical initiating process followed by synthesis of a poly(amidoxime) ligand by oximation reaction. The resulting products were characterized by FT-IR, FE-SEM, EDX, TGA, DSC, and XPS. The poly(amidoxime) ligand was used to coordinate with and extract a series of transition metal ions from water samples. The binding capacity (qe) of the ligand with the metal ions such as copper, iron, cobalt, nickel, and lead were 260, 210, 168, 172, and 272 mg g-1, respectively at pH 6. The adsorption process followed the pseudo-first-order kinetic model (R2 > 0.99) and as well as the Freundlich isotherm model (R2 > 0.99) indicating the occurrence of a multi-layer adsorption process in the amidoxime ligand adsorbent. Results from reusability studies show that the ligand can be recycled for at least 10 cycles without any significant losses to its initial adsorption capacity. The synthesized polymeric ligand was shown to absorb heavy metals from electroplating wastewater with up to 95% efficiency.
The combination of metallic bio-inert material, stainless-steel 316L (SS316L) and a bio-active material, hydroxyapatite (HA) can produce a composite which has superior properties for orthopaedic applications. The main objective of this study is to investigate the effects of sintering temperature and holding time on the physical and mechanical properties of the sintered part. 50wt.% SS316L and 50wt.% HA were mixed with a binder system of palm stearin (PS) and polyethylene (PE) at 61 vol.% powder loading. Rheological properties show a pseudo-plastic behaviour of the feedstock, where viscosity decreases with increasing shear rate. The feedstock was injection moulded into a tensile bar shape while thermal debinding was carried out at 320°C and 500°C. The brown parts were sintered at 1000, 1100, 1200 and 1300°C, with three different sintering times of 1, 3 and 5 hours in the furnace. It was found that the highest sintered density measured was 95.61% of the theoretical density. In addition, the highest hardness and Young's modulus measured were 150.45 HV and 52.61 GPa respectively, which are higher than those of human bone. The lowest percentage of carbon content was 0.022wt.% given by the sample sintered at 1300°C for 1 hour. Therefore, SS316L/HA composite with good mechanical and physical properties was successfully produced through the PIM process.
Electrospun polyhydroxybutyrate (PHB) fibers were dip-coated by polymethyl methacrylate-co-methacrylic acid, poly(MMA-co-MAA), which was synthesized in different molar ratios of the monomers via free-radical polymerization. Fabricated platfrom was employed for immobilization of the dengue antibody and subsequent detection of dengue enveloped virus in enzyme-linked immunosorbent assay (ELISA). There is a major advantage for combination of electrospun fibers and copolymers. Fiber structre of electrospun PHB provides large specific surface area available for biomolecular interaction. In addition, polymer coated parts of the platform inherited the premanent presence of surface carboxyl (-COOH) groups from MAA segments of the copolymer which can be effectively used for covalent and physical protein immobilization. By tuning the concentration of MAA monomers in polymerization reaction the concentration of surface -COOH groups can be carefully controlled. Therefore two different techniques have been used for immobilization of the dengue antibody aimed for dengue detection: physical attachment of dengue antibodies to the surface and covalent immobilization of antibodies through carbodiimide chemistry. In that perspective, several different characterization techniques were employed to investigate the new polymeric fiber platform such as scanning electron microscopy (SEM), atomic force microscopy (AFM), water contact angle (WCA) measurement and UV-vis titration. Regardless of the immobilization techniques, substantially higher signal intensity was recorded from developed platform in comparison to the conventional ELISA assay.
Anodizing could be used for bio-functionalization of the surfaces of titanium alloys. In this study, we use anodizing for creating nanotubes on the surface of porous titanium alloy bone substitutes manufactured using selective laser melting. Different sets of anodizing parameters (voltage: 10 or 20V anodizing time: 30min to 3h) are used for anodizing porous titanium structures that were later heat treated at 500°C. The nanotopographical features are examined using electron microscopy while the bioactivity of anodized surfaces is measured using immersion tests in the simulated body fluid (SBF). Moreover, the effects of anodizing and heat treatment on the performance of one representative anodized porous titanium structures are evaluated using in vitro cell culture assays using human periosteum-derived cells (hPDCs). It has been shown that while anodizing with different anodizing parameters results in very different nanotopographical features, i.e. nanotubes in the range of 20 to 55nm, anodized surfaces have limited apatite-forming ability regardless of the applied anodizing parameters. The results of in vitro cell culture show that both anodizing, and thus generation of regular nanotopographical feature, and heat treatment improve the cell culture response of porous titanium. In particular, cell proliferation measured using metabolic activity and DNA content was improved for anodized and heat treated as well as for anodized but not heat-treated specimens. Heat treatment additionally improved the cell attachment of porous titanium surfaces and upregulated expression of osteogenic markers. Anodized but not heat-treated specimens showed some limited signs of upregulated expression of osteogenic markers. In conclusion, while varying the anodizing parameters creates different nanotube structure, it does not improve apatite-forming ability of porous titanium. However, both anodizing and heat treatment at 500°C improve the cell culture response of porous titanium.
A new sensing area for a sensor based on surface plasmon resonance (SPR) was fabricated to detect trace amounts of mercury and lead ions. The gold surface used for SPR measurements were modified with polypyrrole-chitosan (PPy-CHI) conducting polymer composite. The polymer layer was deposited on the gold surface by electrodeposition. This optical sensor was used for monitoring toxic metal ions with and without sensitivity enhancement by chitosan in water samples. The higher amounts of resonance angle unit (ΔRU) were obtained for PPy-CHI film due to a specific binding of chitosan with Pb(2+) and Hg(2+) ions. The Pb(2+) ion bind to the polymer films most strongly, and the sensor was more sensitive to Pb(2+) compared to Hg(2+). The concentrations of ions in the parts per million range produced the changes in the SPR angle minimum in the region of 0.03 to 0.07. Data analysis was done by Matlab software using Fresnel formula for multilayer system.
In this study, the performance of glyphosate removal in an electrocoagulation batch with two electrodes formed by the same metal type, consisting of aluminum, iron, steel and copper have been compared. The aim of this study intends to remove glyphosate from an aqueous solution by an electrocoagulation process using metal electrode plates, which involves electrogeneration of metal cations as coagulant agents. The production of metal cations showed an ability to bind together to form aggregates of flocs composed of a combination of glyphosate and metal oxide. Electrocoagulation using aluminum electrodes indicated a high percentage removal of glyphosate, 94.25%; followed by iron electrodes, 88.37%; steel electrodes, 62.82%; and copper electrodes, 46.69%. The treated aqueous solution was then analyzed by Fourier Transform Infrared Spectroscopy. Percentages of Carbon, Hydrogen, Nitrogen, Sulfur remaining in the treated aqueous solution after the electrocoagulation process have been determined. The treated water and sludge were characterized and the mechanism of the overall process was concluded as an outcome. An X-Ray Diffraction analysis of dried sludge confirmed that new polymeric compounds were formed during the treatment. The sludge composed of new compounds were also verified the removals. This study revealed that an electrocoagulation process using metal electrodes is reliable and efficient.
Even though drug-eluting stent (DES) has prominently reduced restenosis, however, its complication of delayed endothelialization has caused chronic side effect. A coating of ginseng-based biodegradable polymer could address this issue due to its specific therapeutic values. However, deposition of this type of stable coating on metallic implant often scarce. Therefore, in this study, different polyaniline (PANI) emeraldine compositions were adopted to electrodeposit ginsenoside encapsulated poly(lactic-co-glycolic acid) microcapsules coating. The coating surfaces were analyzed using attenuated total reflectance-Fourier transform infrared spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscopy, contact angle, and atomic force microscopy instruments. A month coating stability was then investigated with an evaluation of in vitro human umbilical vein endothelial cell analyses consisted of cytotoxicity and cells attachment assessments. The 1.5 mg PANI emeraldine has assisted the formation of stable, uniform, and rounded microcapsules coating with appropriate wettability and roughness. Less than 1.5 mg PANI emeraldine was not enough to drive the formation of microcapsules coating while greater than 1.5 mg caused the deposition of melted microcapsules. The similar coating also has promoted greater cells proliferation and attachment compared to other coating variation. Therefore, the utilization of electrodeposition to deposit a drug-based polymer coating could be implemented to develop DES, in accordance to stent implantation which ultimately aims for enrich endothelialization.
Carbon dioxide assisted particle formation combined with electrospraying using supercritical CO2 (scCO2) as an aid (Carbon Dioxide Assisted Nebulization-Electrodeposition, CAN-ED) was used to produce Bortezomib loaded poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) P(3HB-co-3HHx) nanoparticles for sustained release. The morphology and structure of the prepared nanoparticles were investigated by SEM, TEM and FT-IR spectroscopy. Average diameter of particles obtained was 155nm and the average core sizes of P(3HB-co-3HHx) nanoparticles were between 6 and 13nm. The drug loading capacity, drug release and stability of Bortezomib loaded P(3HB-co-3HHx) nanoparticles were analyzed. The maximum loading capacity was achieved at pH=6.0 in phosphate buffer (K2HPO4/KH2PO4). It was found that temperature did not affect the stability of Bortezomib loaded nanoparticles and it was good both at 37°C and 4°C. This study pointed out that CAN-ED is a green method to produce P(3HB-co-3HHx) nanoparticles for pH responsive targeting of Bortezomib especially to parts of the body where size exclusion is not crucial.
This study describes an investigation using tropical water lilies (Nymphaea spontanea) to remove hexavalent chromium from aqueous solutions and electroplating waste. The results show that water lilies are capable of accumulating substantial amount of Cr(VI), up to 2.119 mg g(-1) from a 10 mg l(-1) solution. The roots of the plant accumulated the highest amount of Cr(VI) followed by leaves and petioles, indicating that roots play an important role in the bioremediation process. The maturity of the plant exerts a great effect on the removal and accumulation of Cr(VI). Plants of 9 weeks old accumulated the most Cr(VI) followed by those of 6 and 3 weeks old. The results also show that removal of Cr(VI) by water lilies is more efficient when the metal is present singly than in the presence of Cu(II) or in waste solution. This may be largely associated with more pronounced phytotoxicity effect on the biochemical changes in the plants and saturation of binding sites. Significant toxicity effect on the plant was evident as shown in the reduction of chlorophyll, protein and sugar contents in plants exposed to Cr(VI) in this investigation.