Nickel contamination analysis at cost-effective silver printed paper-based electrodes based on carbon black dimethylglyoxime ink as electrode modifier

Electrochemical detection of metal cations at paper-based sensors has been suggested as an attractive alternative to current spectroscopic and chromatographic detection techniques due to the ease of fabrication, disposable nature, and low cost. Herein, a novel carbon black (CB), dimethylglyoxime (DMG) ink is designed as an electrode modifier in conjunction with 3-electrode inkjet-printed paper substrates for use in the adsorptive stripping voltammetric electroanalysis of nickel cations in water samples. The developed method provides a novel, low-cost, rapid, and portable adsorptive stripping detection approach towards metal analysis in the absence of the commonly used toxic metallic films. The study demonstrated a novel approach to nickel detection at paper-based sensors and builds on previous work in the field of paper-based metal analysis by limiting the use of toxic metal films. The device sensitivity is improved by increasing the active surface area, electron transfer kinetics, and catalytic effects associated with non-conductive dimethylglyoxime films through CB nanoparticles for the first time and confirmed by electroanalysis. The first use of the CB-DMG ink allows for the selective preconcentration of analyte at the electrode surface without the use of toxic Mercury or Bismuth metallic films. Compared to similarly reported paper-based sensors, improved limits of detection (48 µg L-1), selectivity, and intermetallic interferences were achieved. The method was applied to the detection of nickel in water samples well below World Health Organization (WHO) standards.

Influence of Al Doping on the Morphological, Structural and Gas Sensing Properties of Electrochemically Deposited ZnO Films on Quartz Resonators

The detection of hazardous gases at different concentration levels at low and room temperature is still an actual and challenging task. In this paper, Al-doped ZnO thin films are synthesized by the electrochemical deposition method on the gold electrodes of AT-cut quartz resonators, vibrating at 10 MHz. The average roughness, surface morphology and gas sensing properties are investigated. The average roughness of Al-doped ZnO layers strongly depends on the amount of the doping agent Al2(SO4)3 added to the solution. The structural dependence of these films with varying Al concentrations is evident from the scanning electron microscopy images. The sensing properties to ethanol and ammonia analytes were tested in the range of 0–12,800 ppm. In the analysis of the sensitivity to ammonia, a dependence on the concentration of the added Al2(SO4)3 in the electrochemically deposited layers is also observed, as the most sensitive layer is at 3 × 10−5 M. The sensitivity and the detection limit in case of ammonia are, respectively, 0.03 Hz/ppm and 100 ppm for the optimal doping concentration. The sensitivity depends on the active surface area of the layers, with those with a more developed surface being more sensitive. Al-doped ZnO layers showed a good long-term stability and reproducibility towards ammonia and ethanol gases. In the case of ethanol, the sensitivity is an order lower than that for ammonia, as those deposited with Al2(SO4)3 do not practically react to ethanol.

Preparation of a Photosensitive Composite Carbon Fiber for Spilled Oil Cleaning

This paper deals with preparing a functional composite carbon fiber with a large surface area for spilled oil cleaning. The composite fiber consisted of photosensitive oxide particles and polymer-derived carbon. It was made by co-spinning the polymer and metallic compounds. After heat treatment at high temperatures, an activated carbon fiber containing oxide particles was obtained. The particles were found distributed in the fiber and at the surface of the fiber. The composite fiber was found sensitive to sunlight. Fiber mats made of the composite fiber possessed a high surface area for oil absorption and removal. Cobalt(II) titanate particles were obtained from the reaction of titanium dioxide and cobalt oxide. The reaction happened in situ through the hydrolysis of metallic compounds in the spun fiber. The titanium dioxide and cobalt(II) titanate particle-containing fibers demonstrated the photoactivity in the visible light spectrum. It was concluded that particle-containing composite carbon fiber mats can be prepared successfully by co-electrospinning. Due to the oleophilic property and the high active surface area, the composites are suitable for spilled oil cleaning through fast absorption.

A Low Cost Fe3O4–Activated Biochar Electrode Sensor by Resource Utilization of Excess Sludge for Detecting Tetrabromobisphenol A

Owing to its ubiquity in natural water systems and the high toxicity of its accumulation in the human body, it is essential to develop simple and low-cost electrochemical sensors for the determination of 3,3′,5,5′-tetrabromobisphenol A (TBBPA). In this work, Fe3O4–activated biochar, which is based on excess sludge, was prepared and characterized using scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS), Fourier transform infrared spectroscopy (FTIR) and BET analysis to analyze its basic features. Subsequently, it was used to fabricate an electrochemical sensor for the detection of TBBPA. The electrochemical test results revealed that the Fe3O4–activated biochar film exhibited a larger active surface area, a lower charge transfer resistance and a higher accumulation efficiency toward TBBPA. Consequently, the peak current of TBBPA was significantly enhanced on the surface of the Fe3O4–activated biochar. The TBBPA sensing platform developed using the Fe3O4–activated biochar composite film, with relatively a lower detection limit (3.2 nM) and a wider linear range (5–1000 nM), was successfully utilized to determine TBBPA levels in water samples. In summary, the effective application of Fe3O4–activated biochar provided eco-friendly and sustainable materials for the development of a desirable high-sensitivity sensor for TBBPA detection.

Improving Catalytic Activity in the Electrochemical Separation of CO2 Using Membrane Electrode Assemblies

The direct electrochemically driven separation of CO2 from a humidified N2, O2, and CO2 gas mixture was conducted using an asymmetric membrane electrode assembly (MEA). The MEA was fabricated using a screen-printed ionomer bound Pt cathode, an anion exchange membrane (AEM), and ionomer bound IrO2 anode. Electrocatalyst materials were physically and chemically characterized prior to inclusion within the electrode. Electrochemical impedance spectroscopy (EIS) and linear sweep voltammetry (LSV) measurements using a rotating disk electrode (RDE) were used to quantify the catalytic activity and determine the effects of the catalyst-to-ionomer ratio. Catalysts were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer–Emmett–Teller (BET) surface analysis, and (dynamic light scattering) DLS to evaluate catalyst structure, active surface area, and determine the particle size and bulk particle size distribution (PSD). The electrocatalyst layer of the electrodes were fabricated by screen printing a uniformly dispersed mixture of catalyst, dissolved anionic ionomer, and a solvent system onto an electrode supporting gas diffusion layer (GDL). Pt IrO2 MEAs were fabricated and current-voltage relationships were determined using constant-current measurements over a range of applied current densities and flow rates. Baseline reaction kinetics for CO2 separation were established with a standard set of Pt-IrO2 MEAs.

Hydrothermal Carbonization of Waste Sugarcane Bagasse for the Effective Removal of Emerging Contaminants from Aqueous Solution

Porous carbon spheres were fabricated from sugarcane bagasse using a sustainable hydrothermal carbonization process followed by alkali impregnation inert atmosphere activation. Developed spheres were technically analysed for their chemical science, structural morphology, texture, porosity with respect to size distribution, and thermal degradation. Spheres are functionally enriched with oxygenated groups showing amorphous nature portraying as a smooth surface. After activation, intensity of functional groups is reduced due to reduction reaction by KOH thereby yielding highly rich porous carbon. The active surface area developed on spheres is 111 m2 g-1 holding pores that are mesoporous in nature. Resistance to thermal exposure using TGA showed that decomposition of hemicelluloses followed by cellulose yielded aromatized carbon-rich skeleton through thermal degradation of carboxyl and hydroxyl groups. Developed carbon was found to be effective in removing Ciprofloxacin Hydrochloride from water with maximum adsorption capacity of 110.008 mg g-1. Mechanistic removal followed pseudo-second-order kinetics along with Freundlich mode of adsorption. The presence of carboxylic and hydroxyl groups in porous carbon favoured elimination of CPF from water. The development of HTC-derived carbon helped conserving the energy thereby reducing the cost requirement.

Preparation of Very Thin Zinc Oxide Films by Liquid Deposition Process: Review of Key Processing Parameters

We used sol-gel and spin-coating in the original configuration of a liquid deposition process to synthesize particularly thin ZnO films (<100 nm) with nano-granular morphology, high grain orientation and variable optical properties. The concentration of the zinc salt, the concentration of the chelating agent, the nature of the solvent and the substrate material have been identified as key parameters that determine the microstructure of the deposited layer and thus its final properties. The thorough and practical examination of the effects of the synthesis parameters evidenced a three-step growth mechanism for these ZnO thin films: (i) a reaction of precursors, (ii) a formation of nuclei, and (iii) a coalescence of nanoparticles under thermal annealing. The growth of these very thin films is thus conditioned by the interaction between the liquid phase and the substrate especially during the initial steps of the spin coating process. Such thin ZnO films with such nano-granular morphology may be of great interest in various applications, especially those requiring a large active surface area.

Single step polyol synthesis of highly stable Pt/C/SiO2 catalysts for use in PEMFCs: effects of pH, temperature and W/EG ratio

Hybrid supports have been proposed as a new alternative to increase the stability of ORR catalysts used in PEMFCs for automotive applications since they are known to be stable under harsh conditions. In this work, Pt nanoparticles were deposited over C/SiO2, via single-step polyol method, to take advantage of the corrosion-resistance properties of silica nanoparticles. In fact, the synthesis parameters, namely, pH, temperature, and glycol concentration had a remarkable impact on the Pt size-distribution, crystallinity, and dispersion over the C/SiO2 supports. A maximum ORR activity and stability was obtained for Pt/C/SiO2 catalysts produced at 1:6 W/EG (v/v). The addition of SiO2 nanoparticles to the carbon structure showed their ability to effectively inhibit support corrosion and Pt nanoparticles detachment and/or growth, with the pH adjustments being critical for obtaining highly stable C/SiO2 supports. Pt/C/SiO2 synthetized under acidic conditions revealed the highest stability when subjected to accelerated stress tests (ASTs), losing only 30 % of the initial electrochemically active surface area (ECSA) of Pt after 4 000 cycles from 0.6 to 1 V (vs RHE), whereas the commercial Pt/C revealed > 50 % of ECSA loss.

Electrocatalytic performance of sonochemically synthesized Pt–Ni/C nanoparticles in fuel cell application

Developing high-performance electrocatalysts using simple and controllable methods is of interest to reduce the cost of polymer electrolyte membrane fuel cells. In this study, platinum is alloyed with nickel and supported on carbon (Pt–Ni/C) via an ultrasound-assisted route. The crystallite and particle sizes of the obtained nanoparticles were smaller than the commercial carbon-supported Pt nanoparticles. The sonochemically synthesized Pt–Ni/C nanoparticles exhibited superior electrocatalytic properties than the commercial Pt/C nanoparticles in the fuel cell operation. Electrochemical measurements performed with Pt–Ni/C electrocatalyst displayed excellent oxygen reduction and higher electrochemical active surface area (EASA). Optimum fuel cell performance based on peak power density using Pt–Ni/C electrocatalyst was observed as 0.28 W/cm2 at 0.39 V.

Controllable morphology of Bi2S3 nanostructures formed via hydrothermal vulcanization of Bi2O3 thin-film layer and their photoelectrocatalytic performances

Bi2S3 nanostructures with various morphologies were synthesized through hydrothermal vulcanization at different sulfur precursor (thiourea) concentrations. A 100 nm thick sputter-deposited Bi2O3 thin-film layer on a fluorine-doped tin oxide glass substrate was used as a sacrificial template layer. The etching of the Bi2O3 sacrificial template layer and the regrowth of Bi2S3 crystallites during hydrothermal vulcanization produced the different Bi2S3 nanostructure morphologies. The lowest sulfur precursor concentration (0.01 M) induced the formation of Bi2S3 nanosheets, whereas the Bi2S3 nanoribbons and nanowires were formed with increased sulfur precursor concentrations of 0.03 and 0.1 M, respectively. These results indicate that sputter-deposited Bi2O3 thin-film layers can be effectively used to form low-dimensional Bi2S3 crystals with controllable morphologies. Among the various Bi2S3 samples, the Bi2S3 nanosheets exhibited superior photoactive ability. The higher active surface area, surface defect density, light absorption capacity, and photo-induced charge separation ability of Bi2S3 nanosheets explain their superior photoelectrocatalytic degradation ability of rhodamine B dyes.