Cyclic Voltammetry Measurements Research Articles

The effect of solvent type and composition on the synthesis of boron-doped ordered mesoporous carbons

Boron-doped ordered mesoporous carbons (B-OMCs) were synthesized using different solvent types and compositions to study the effect of the solvent medium on the physical properties and oxygen reduction activities of the resultant structures. Materials were synthesized by a one-pot self-assembly method, using resorcinol and formaldehyde as carbon source, boric acid as boron source and triblock copolymer Pluronic F127 as the structure directing agent. Different solvents, namely ethanol, n-propanol, isopropanol and acetone were used as solvent media along with water as the cosolvent. Among different solvents, ethanol and n-propanol gave better-ordered structures and also had higher surface areas. At this stage, the highest boron doping percentage was obtained as 1.38 % with n-propanol. In the second stage, B-OMCs were synthesized with n-propanol in different water/n-propanol (W/N) molar ratios varying between 2.5 and 4.75. The orderliness was observed to be better in samples with low W/N ratios of 2.5 and 3.25 and the morphologies shifted from 2D to 3D interconnected type with the increase of water content. The average pore sizes of samples varied between 7.9 and 9.7 nm. On the other hand, the highest surface area (729 m2/g) and the highest boron doping percentage (1.53 %) were obtained with the W/N ratio of 4. XPS analysis showed that 23 % (w/w) of doped boron in this sample was in substitutional state while the remaining boron was found in mixed B–C and B–O states. Cyclic voltammetry measurements for the samples with W/N ratios of 2.5, 3.25 and 4 showed significant oxygen reduction activities at −0.28 and −0.29 V. Results showed that the properties of solvent play an effective role in the orderliness, pore structure and surface composition of B-OMCs, which in turn affect their electrochemical properties. Among different types of solvents, n-propanol can be used as an alternative to ethanol with the W/N ratio of 4 giving the highest surface area and boron doping percentage.

Electrochemical reduction processes and extraction of titanium with different valence states in molten CaO-CaF2 slags

Titanium is an excellent structural and functional material. At present, the production of titanium has long process cycle, high energy consumption, serious pollution and other characteristics, so the development of low-cost titanium production methods has extremely far-reaching significance. In this work, the electrochemical reduction process of Ti(IV) and Ti(II) in the CaF2-CaO melt were investigated by cyclic voltammetry and square wave voltammetry measurements at 1740 K, respectively. In the CaF2-CaO-5 wt% TiO2 melt, Ti(IV) ions were reduced to Ti by one step. One measure was taken to lower the valence state of Ti ions: Ti(IV) ions in the melt was changed to Ti(II) by adding Ti0. Ti(IV) ions were reduced in two steps: in the CaF2-CaO-5 wt% TiO2-Ti0 melt, Ti(IV) → Ti(II) and Ti(II) → Ti, respectively, and in the CaF2-CaO-5 wt% TiO, the Ti(II) ions were reduced in a single step: Ti(II) → Ti. It was found that both migration and mass transfer affected the reduction processes. In contrast to the Ti(IV) reduction to Ti process, the Ti(II) reduction to Ti process showed a higher diffusion rate. Electrolytes and electrodes were analyzed after titanium electrodeposition by XRD. It was found that there were no metal titanium was detected in the electrolyte placed close to the cathode after electrodeposition. It believed that the formed metallic Ti reacted with dissolved O2- in the melt to form TiO. The reduction process of Ti(IV) on the iron electrode was investigated, the metal Ti was reduced by alloying process, the oxidation of Ti was hindered, there was a dense structure layer of CaTiO3 outside the reduced metal Ti that prevented the ions transfer and affected the Ti(IV) ions migration process, which might be the main factor that the Ti(IV) reduction process was controlled by migration. The lower valence state of Ti in the melt promoted the formation of Ca2TiO4, which increased the ion migration rate and decreased the mass transfer rate. It was suggested that titanium or titanium alloys may be prepared by reducing the valence of Ti(IV) in minerals and altering the melt composition. It is feasible to prepare titanium and titanium alloys by MOE short process using ore as raw material.

Light-enhancing ketone transfer hydrogenation catalyzed by diphosphine phenanthroline ruthenium complexes

The cationic phenanthroline ruthenium derivatives [Ru(OAc)(dppb)(NN)]OAc (NN = phen 1, imidazo[4,5-f][1,10]phenanthroline 2) have been obtained in high yield by reaction of the acetate [Ru(OAc)2dppb] with the corresponding NN ligand. The dinuclear cyclometalated [(dppb)(η2-OAc)(Ru(µ-NN-phenimid-NC)Ru(η2-OAc)(dppb)]OAc (3) has been prepared from 2 with [Ru(OAc)2(dppb)] via elimination of acetic acid. The characterization of these compounds has been carried out by NMR, FT-IR, UV–Vis, conductivity and cyclic voltammetry measurements. These derivatives display catalytic activity in the transfer hydrogenation of aromatic and aliphatic cyclic ketones at S/C up to 2000 in presence of NaOiPr in 2-propanol. An increase of the rate (up to 8 times) has been observed upon irradiation at 30 and 60 °C (300 W Xenon Arc Lamp light source). Control experiments show that [Ru(OiPr)2(dppb)(phen)] (1A), formed from 1 by substitution of the acetate with the isopropoxide ligand, shows a stronger emission compared to 1 and that 1A is quenched by NaOiPr, affording the dihydride [Ru(H)2(dppb)(phen)] (1C) via a photo induced β-H elimination.

Purification of Spherical Graphite as Anode for Li-Ion Battery: A Comparative Study on the Purifying Approaches.

Graphite is a versatile material used in various fields, particularly in the power source manufacturing industry. Nowadays, graphite holds a unique position in materials for anode electrodes in lithium-ion batteries. With a carbon content of over 99% being a requirement for graphite to serve as an electrode material, the graphite refinement process plays a pivotal role in the research and development of anode materials for lithium-ion batteries. This study used three different processes to purify spherical graphite through wet chemical methods. The spherical graphite after the purification processes was analysed for carbon content by using energy-dispersive X-ray (EDX) spectroscopy and was evaluated for structural and morphological characteristics through X-ray diffraction (XRD), scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) analyses. The analyses results indicate that the three-step process via H2SO4-NaOH-HCl cleaning can elevate the carbon content from 90% to above 99.9% while still maintaining the graphite structure and spherical morphology, thus enhancing the surface area of the material for anode application. Furthermore, the spherical graphite was studied for electrochemical properties when used as an anode for Li-ion batteries using cyclic voltammetry (CV) and galvanostatic charge-discharge (GCD) measurements. The results demonstrated that the purification process significantly improves the material's capacity with a specific capacity of 350 mAh/g compared to the 280 mAh/g capacity of the anode made of spherical graphite without purification.

Simultaneous Determination of Chemical Oxygen Demand, Total Nitrogen, Ammonia, and Phosphate in Surface Water Based on a Multielectrode System.

A technique for monitoring chemical oxygen demand (COD), total nitrogen (TN), ammonia (N-NH4), and phosphate (P-PO4) in surface water with a targeted signal multielectrode system (Cu, Ir, Rh, Co(OH)2, and Zr(OH)4 electrodes) is proposed for the first time. Each water quality index is specifically detected by at least two electrodes with distinct selectivity sensing mechanisms. Cyclic voltammetry and electrochemical impedance measurements are employed for multidimensional signal acquisition, complemented by normalization and Least Absolute Shrinkage and Selection Operator (LASSO) for principal feature extraction and dimension reduction. Multiple linear regression (MLR), partial least-squares (PLS), and eXtreme Gradient Boosting (XGBoost) were employed to evaluate the established prediction model. The precisions of the multielectrode system are ±10%/±5 ppm of COD, ±10%/±0.2 ppm of TN, ±5%/±0.1 ppm of N-NH4, and ±5%/±0.01 ppm of P-PO4. The analysis time of the multielectrode system is reduced from hours to minutes compared with traditional analysis, without any sample pretreatment, facilitating continuous online monitoring in the field. The developed multielectrode system offers a feasible strategy for online in situ monitoring of surface water quality.

Pulsed galvanostatic electrodeposition of tellurium nanostructures on stainless steel from copper anode slimes plating bath: Effect of pulse parameters

The electrochemical behavior of Te in alkaline media was determined by cyclic voltammetry and linear sweep voltammetry measurements. It indicated that TeO32− ion was first reduced to Te(s), then to Te22− ion. For the first time, the pulsed electrodeposition of tellurium on stainless steel has been studied in an alkaline bath and the effect of duty cycle, frequency, and current density on current efficiencies and morphology were indicated at room temperature. Pulse duty cycles ranging from 10 to 75%, frequencies ranging from 10 to 100 Hz, and current densities ranging from 7.5 to 30 mA/cm2 were employed. The morphology of the electrodeposition of tellurium samples was characterized by SEM. The results showed that due to increasing side reactions at higher current density, the current efficiency decreased with increasing current density. The results of Scanning Electron Microscopy (SEM) cleared that more compact structures with lower porosity were observed for the electrodeposits at lower current densities and less compact samples were obtained at higher current densities. It has been found that the current efficiency of tellurium plating decreases as the pulse duty cycle increases from 10% to 75%. Maximum current efficiency has been observed at 10% duty cycle. The study of the effect of duty cycle on morphology showed that the samples synthesized at a duty cycle of 10% and 25% have approximately similar appearance and particle size. With more increasing of duty cycles to 50 and 75% due to increasing hydrogen evolution rate and H2 bubbling at the electrode surface the morphology has been changed remarkably. The current efficiency of the deposit tellurium exhibited a strong dependence on the frequency. As frequency increases, the current efficiency almost decreases. In most cases, the maximum current efficiency is obtained at a 10 Hz frequency. The study of the effect of frequency on morphology showed that hydrogen evolution plays a significant role in the morphology formation of samples obtained at low pulse frequency (10 Hz), two processes of hydrogen evolution and anisotropic growth have key roles in morphology formation at medium pulse frequency (50 Hz) and anisotropic growth is the mechanism of morphology formation at high pulse frequency (100 Hz).

P-EcStat: A Versatile Design of Photoelectrochemical and Electrochemical Sensing System with Smartphone Interface via Bluetooth Low Energy

Electrochemical and photoelectrochemical sensors are a rapidly developing field in analytical chemistry. However, commercial systems often lack versatility and affordability, hindering wider adoption. Additionally, the absence of integrated excitation light sources limits their application in photoelectrochemical sensing. Here, we present a highly precise, versatile, affordable measurement system for both electrochemical and photoelectrochemical sensing applications. The system incorporates a three-electrode potentiostat with a synchronized excitation light source. This design enables the system to perform conventional electrochemical measurements like cyclic voltammetry, chronoamperometry, and photoelectrochemical amperometric measurements with controlled light excitation. The developed measurement system operates within a voltage range suitable for a measurable current range of 1 nA to 18 mA, with a high precision of 99%. The excitation source is a monochromatic LED system offering seven distinct wavelengths with digitally controlled intensity via a digital-to-analog converter. Furthermore, an Android-based user interface allows wireless system control via Bluetooth Low Energy. The report also details the construction of a photoelectrochemical experiment using copper (II) oxide nanorods synthesized by the hydrothermal process as the photoactive material employed to test the experiment on a potassium ferricyanide/potassium ferrocyanide solution. This user-friendly system allows broader exploration of electrochemical and photoelectrochemical sensing applications.

A novel electroactive biopolymer-graphene oxide nanocomposite membrane for high-performance electrochemical sensing of ethylene

This study focuses on formulating an electroactive composite membrane using polyvinyl alcohol (PVA), chitosan (CHT), and graphene oxide (GO), specifically emphasizing its application in electrochemical ethylene detection. Through the surface functionalization of the PVA-CHT-GO membrane via GO activation, the nanocrystallite GO-based composite, when incorporated into a microelectrode chip, exhibited a transformative enhancement in electrochemical ethylene sensing. Comprehensive characterizations of both the synthesized GO and the PVA-CHT-GO composite membranes were conducted by employing X-ray Diffraction (XRD), Fourier Transform Infrared spectroscopy (FTIR), Raman spectroscopy, Energy Dispersive X-ray spectroscopy (EDS), Field emission scanning electron microscopy (FE-SEM), and Thermal gravimetric analysis (TGA). The XRD pattern provides insights into the stacking height, interplanar spacing, and the number of layers along the (002) direction. The synthesized GO's average nano-crystallite size was determined to be 10.38 nm. The Raman spectrum revealed prominent D and G bands at 1353 and 1591 cm-1, respectively. FE-SEM images depicted the overlapping of GO nanolayers, each layer having a thickness in the range of 20–30 nm. Following surface activation, thin layers developed on the membrane surface, with numerous folds accumulating, exhibiting thickness in the range of 20–50 nm. The intricate characterization underscored the structural and morphological features of the membrane, enhancing our understanding of its surface properties. The effectiveness of ethylene detection using the GO-activated PVA-CHT-GO membrane was evaluated via cyclic voltammetry (CV) measurements. These measurements confirmed the membrane's efficiency, demonstrating ultra-sensitive ethylene detection, even upon initial exposure to ethylene.

Nitrogen-functionalized catalyst synthesized using spent coffee ground biochar-cobalt hybrid for oxygen reduction reaction via pyrolysis and ball-milling

In this work, oxygen reduction reaction (ORR) catalysts were developed from a precursor of spent coffee ground-based biochar. Nitrogen doping was achieved via urea addition preceding a pyrolysis synthesis process, yielding nitrogen-doped biochar (NDB). Cobalt was deposited onto the NDB surface using a non-conventional ball-milling procedure. The microstructure of the synthesized samples was studied through Scanning Electron Microscopy (SEM), where a rather distorted surface, highlighted by prominent wrinkles (which doubled the surface area at 50.58 m2/g), was shown for nitrogen-doped samples. Moreover, the high energy ball-milling technique shows an almost perfect coverage of cobalt nanoparticles on the biochar surface through SEM/EDS and Raman results. Additionally, electrochemical testing was conducted using cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). Cyclic voltammetry measurements conducted under nitrogen (inert) and oxygen-saturated alkaline solution (0.1 M KOH) conditions showed that nitrogen doping enhances the oxygen reduction reaction current (-1 vs -0.59 mA.cm−1 at -0.3 V vs Hg/HgO) and slightly reduces the onset potential compared to pristine biochar. Depositing cobalt onto the NDB surface had a minor adverse effect on the onset potential, but significantly increased the oxygen reduction reaction current, reaching a value of -2.09 mA.cm−2 at -0.3 V vs Hg/HgO. All catalysts were compared to a commercial carbon supported platinum catalyst (Pt10%C) to showcase the potential room of improvement for the developed catalysts.

Copper (II) complexes based on the mixed ligand system: Study of synthesis, characterization, and stopped‐flow kinetics of copper oxidase‐mimicking catalytic activity

Two copper (II) complexes based on the mixed ligand system were synthesized and structurally characterized. The molecular formulae for complex (1), [Cu2L1L′] and complex (2), [CuL2L′] were determined based on analytical data, molar conductance, and thermal analysis results. The optimized structures of complexes (1) and (2) were determined by magnetic and spectroscopic measurements (FTIR, UV–Vis, and ESR) and confirmed by processing powder X‐ray diffraction data by Expo 2014 software. The geometry index (τ5), determined by ESR spectra and structural analysis based on powder X‐ray, demonstrates the square pyramidal geometry of the Cu (II) center of [Cu2L1L′] and [CuL2L′]. Cyclic voltammetry measurements were performed to elucidate the relationship between the redox properties of (1) and (2) and their oxidase‐mimicking catalytic activity. Catalytic aerobic oxidation of the polyphenols 3,5‐di‐tert‐butylcatechol (3,5‐DTBCH2), 4‐nitrocatechol, and 2‐aminophenol (2‐APH3) was studied by stopped‐flow technique. Promising catechol oxidase (COX) and phenoxazinone synthase (PHS) mimetic activity have been demonstrated for (1) and (2). Electrochemical data were used to determine the free energy (ΔG°) or driving force (−λ), and their correlation with the oxidase mimetic activity of(1) and (2) was examined. Several experimental procedures have been performed that have helped describe the catalytic mechanisms of the catalytic reactions taking place.

Using anodic oxidation for boosting supercapacitive performance of thermally-oxidized cobalt coatings with various morphologies

Metal oxide electrodes for supercapacitors are commonly synthesized through the hydrothermal method. Despite the simplicity and cost-effectiveness of electrodeposition for producing electrode materials, there is a scarcity of literature on electrodeposited electrodes. Previous studies have utilized nitrate-based solutions and subsequent heat-treatment to fabricate these materials without additional treatments to enhance their performance. This research explores the creation of cobalt coatings with varying morphologies (pyramidal, ridge-shaped, powdery, and rough nodular) using electrodeposition from sulfate-based solutions by adjusting deposition parameters. The cobalt coatings were then heat-treated at 550˚C for 3 h to convert them to cobalt oxide, a promising material for supercapacitor electrodes. The study investigates the impact of initial morphology on the structure, phases formed, and supercapacitive properties of the heat-treated coatings. Analysis of XRD and FTIR data indicated that the primary phase post-heat treatment was Co3O4, alongside some CoO. Cyclic voltammetry (CV) measurements in 1 M KOH solution revealed that the powdery coating exhibited the highest specific capacitance of 796±21 mF cm−2 (∼110 F g−1) at a scanning rate of 2 mV s−1, surpassing the heat-treated pyramidal coating by approximately tenfold. These CV findings were corroborated by galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS) analyses. Furthermore, the heat-treated coatings underwent anodic oxidation in a 3 M KCl solution for 5 minutes to assess the impact of this lesser-known process on their capacitive behavior. Following anodic oxidation, the ridge-shaped and pyramidal coatings displayed significantly enhanced specific capacitance due to the formation of fine pores and surface modifications. Specifically, the specific capacitance of the ridge-shaped coating surged from 103±4 mF cm−2 (∼11 F g−1) to 1832±64 mF cm−2 (∼201 F g−1) at a scanning rate of 2 mV s−1 after anodic oxidation. Although the rough nodular coating also experienced an increase in specific capacitance, the morphology and electrochemical characteristics of the powdery coating remained relatively stable throughout the study.

Synthesis of carbazole-based Schiff base and fluorescence turn on sensor sensitive to Cr3+ ion: Oxidative and electrochemical polymerization and investigation of electrochromic properties

In this study, a Schiff base monomer (ECBA) was initially synthesized from condensation reaction of 3-amino 9-ethyl carbazole (AEC) with 2,4-dihydroxy benzaldehyde (DHBA). Then, its poly(ECBA-1) polymer was synthesized via oxidative polycondensation in methanol/THF (v/v:4/1) medium by NaOCl oxidant. The structures of the obtained monomer and poly(ECBA-1) were confirmed by 1H NMR, 13C NMR and FT-IR. The optical and electrochemical properties of compounds were examined by UV–Vis, fluorescence spectroscopy and cyclic voltammetry (CV) measurements, respectively. The Highest occupied molecular orbital (HOMO), lowest unoccupied molecular orbital (LUMO) energy levels and electrochemical (E’g) and optical band gap (Eg) values were determined for monomer and polymer compounds by cyclic voltammetry and UV–Vis spectrophotometry. Thermal stabilities of the monomer and poly(ECBA-1) were determined from thermogravimetric-differential thermal analysis (TG-DTA) measurements. The molecular weight distribution and Tg temperature of the poly(ECBA-1) were determined by gel permeation chromatography (GPC) and differential scanning calorimetry (DSC) measurements, respectively. The surface morphologies of the synthesized polymers and copolymer were investigated by scanning electron microscopy (SEM). By fluorescence titration, ECBA was found to be selective towards Cr3+ ion among Ag+, K+, Mn2+, Hg2+, Co2+, Ca2+, Ni2+, Cu2+, Zn2+, Pb2+, Cd2+, Fe3+, Cr3+, Cr+6 ions. The selectivity of Cr3+ion was confirmed by the absence of interference from other competitive cationic species. The limit of detection (LOD) and binding constant (Ka) values for the fluorescent probe were calculated as 6.07 x 10-7 M and 1.25 x 104 M−1, respectively. In addition, homopolymer and copolymer synthesis was carried out on Pet ITO selected as working electrode via electropolymerization method by the synthesized ECBA monomer. Homopolymer synthesis was carried out by Cyclic Voltammetry (CV) method and copolymer synthesis was carried out by batch electrolysis method using EDOT with ECBA monomer. Spectroelectrochemical measurements were taken to investigate the electrochromic properties of the prepared homopolymer poly(ECBA-2) and copolymer (Poly(ECBA-co-EDOT)). The copolymer was found to have a more stable structure than the homopolymer.

Synergistic electrochemical and optical properties of a UVC class quaternary nanocomposite incorporating graphene oxide and samarium chromium oxide perovskite

This research presents a comprehensive investigation into a novel quaternary nanocomposite comprising graphene oxide (GO), samarium chromium oxide perovskite (SmCrO3), silicon dioxide (SiO2), and tin dioxide (SnO2). The nanocomposite was synthesized using a modified Stöber method. In order to assess its potential applications in supercapacitors and UVC devices, an extensive analysis of its electrochemical and optical properties was conducted. The crystal structure and phase identification were analyzed using X-ray diffraction (XRD) and Rietveld refinement with X'pert HighScore Plus software, confirming the successful formation of the nanocomposite. Scanning electron microscopy (SEM) provided valuable insights into the structural morphology, while energy dispersive X-ray spectroscopy (EDS) confirmed the presence of constituent elements. Fourier transform infrared (FTIR) analysis and Raman Spectroscopy elucidated the functional groups and chemical bonds, confirming the successful synthesis of the nanocomposite. UV–Vis spectroscopy and photoluminescence (PL) spectroscopy revealed its strong UV radiation absorption and intensified fluorescence properties and confirming the band gap of SmCrO3 and GO/SmCrO3/SiO2/SnO2 quaternary nanocomposite as ∼5.4 eV and 4.84 eV respectively. The potential of nanocomposite potential as a supercapacitor material was evaluated through cyclic voltammetry (CV) measurements and electrochemical impedance spectroscopy (EIS) analyses. Remarkably, the specific capacitance of the nanocomposite reached 253.75 Fg−1 at a scan rate of 10 mVs−1, and electrochemical surface area of 507 cm2, highlighting its exceptional charge storage capability and promising prospects for high-performance energy storage devices. This comprehensive study addresses a significant knowledge gap, providing a profound understanding of the electrochemical and optical behavior of the quaternary nanocomposite. The observed exceptional results underscore its suitability for supercapacitor applications and expected favorable material for UVC device technologies.

Electrochemical degradation of carbamazepine in water by a flow-through and pilot-scale reactor with carbon felt electrodes: Parametric study under realistic operational conditions

Carbamazepine (CBZ) is one of the most stable pharmaceutical compounds that is commonly found in the effluents of wastewater treatment plants (WWTP). In this context, this contribution presents a comprehensive analysis of the different operating parameters of a flow-through and pilot-scale cylindrical reactor for hydrogen peroxide (H2O2) generation, in which the degradation of CBZ takes place. The electrochemical system was evaluated using 8 L of electrolytes prepared with tap water in the presence of methanol as dissolved organic matter or spiked tertiary WWTP effluent, at a volumetric flow of 7 L min−1. This reactor (i) improves the mass transport due to its flow-through configuration using fibrous quasi-three-dimensional carbon felt electrodes, (ii) operates without an external oxygen supply to promote the H2O2 electrosynthesis because it is incorporated by a jet aerator (iii) achieves the Fenton reaction at circumneutral pH due to Fe(II) disposition from a cation exchange resin. At first, the carbonaceous materials were electrochemically characterized by cyclic voltammetry measurements. Different operating parameters were evaluated by factorial design methodologies for H2O2 generation, energetic consumption and CBZ removal. The application of a current density of 1.4 mA cm−2, in a cathode-anode-cathode arrangement immersed in a 120 mM ionic strength solution, allowed to obtain up to 6.4 mg H2O2 L−1 after 40 min, consuming 0.44 kWh m−3. Later, the Fenton reaction was validated by a florescence study, and by the incorporation of 0.75 g of granular activated carbon and 5 g of Fe(II) loaded resin, CBZ abatement yields of 68 % and 32 % were obtained using a synthetic solution and a spiked tertiary WWTP effluent, respectively, and up to 28 % of the dissolved total organic carbon was removed. Finally, an analysis of the stability of the carbon felt electrodes was tackled using scanning electron microscopy and energy-dispersive X-ray spectroscopy.

Glass-sulfur composite cathodes: A new strategy for improving the performance of lithium-sulfur batteries

In this study, we investigated the potential of glass-sulfur composites to improve lithium–sulfur battery (LSB) performance. Glass-sulfur composites were prepared by the precipitation method, and the effect of varying carbon black content was studied. The results showed that glass addition improved the battery performance due to the high ion-conductivity of its structural motif. The 75 % glass variant demonstrated the best results, in both the low carbon and high carbon cases. The cyclic voltammetry (CV) and electrical impedance spectroscopy (EIS) measurements showed that glass-sulfur composites had lower resistivity than pure sulfur, which was beneficial for battery performance. The XANES analysis revealed that the incorporated glass interacted with and modified the properties of sulfur, leading to a higher proportion of sulfur in the -1 oxidation state (S−1). This suggests that the high proportion of S−1 phase benefitted battery capacity. Overall, glass-sulfur composites prepared using the precipitation method and incorporating a high content of carbon show promise as a novel and improved cathode material for LSBs.

Influence of electrophoretic deposition of micro- or nanosized silica particles on the microstructure of carbon fibers and their bond behavior with cementitious matrices

The application of carbon fiber (CF) reinforced cementitious composites is often restricted by the poor load transfer between the components. In this study, two reactive coating materials—nano-silica and micro-silica—are utilized to modify the CF surfaces via an electrophoretic deposition approach. These negatively charged particles are able to be electrosorbed onto the fiber surfaces under a constant electrical field according to the zeta and cyclic voltammetry measurements. After surface treatment, XRD analysis of CFs showed an increase in graphite crystallite thickness and decrement in interlayer spacing d002\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$${d}_{002}$$\\end{document}, significantly affecting the fiber diameters. Additionally, the lengths of crystallites were reduced, which can impair the fiber strength and their temperature stability. Single fiber pullout tests exhibited that the interfacial bonding can be clearly enhanced by both reactive coatings. Microscopic observation revealed that C–S–H gel and calcite structures can be formed near the fiber surfaces after immersion in cement pore solution owing to pozzolanic reaction and nucleation effect, tremendously heightening both chemical and mechanical interaction between fiber and cement. Finally, based on a detailed micromechanical analysis, the reinforcing mechanisms between the differently modified fibers and the cementitious matrix were elaborated and discussed.Graphical abstract

Tributyl(hexyl)phosphonium chloride as a new leveler for microvia copper superconformal electronic plating

A phosphorus-containing new compound of tributyl(hexyl)phosphonium chloride (TBHP), but not the commonly used nitrogen-containing heterocycles and quaternary ammonium salts, is successfully applied for the superconformal copper filling of microvia in acid sulfate electroplating bath for the application of electronic industry. The molecular interaction mechanisms of TBHP combined with suppressor (polyethylene glycol, PEG) and accelerator (bis-(sodium sulfopropyl)-disulfide, SPS) are investigated in detail. Galvanostatic measurements at platinum rotation disk electrode indicate that the leveler of TBHP among with the suppressor and accelerator behaves the key characters of inhibition and convection-dependent adsorption during copper ions electroreduction for the bottom-up filling of microvia. Cyclic voltammetry measurements and in-situ FTIR spectroscopy further reveal that TBHP synergistically interacts with the suppressor to inhibit copper ions electroreduction at the mouth of microvia; while TBHP competes for adsorption with the accelerator, behaving as TBHP gradually replaced by the accelerator at the bottom. Based on the sufficient theoretical supports, the practical copper electroplating is conducted for the verification of microvia void free filling. In the developed novel copper plating formula containing TBHP, PEG and SPS, the void free filling is successfully achieved and the filling percentage (FP) is high in 95.5%.

A novel in-house built printed circuit board-ceria based electrochemical device for rapid detection of Epithelial Sodium Channel (ENaC), a hypertension biomarker

The Epithelial Sodium Channel (ENaC) is a protein that plays a role in the cellular intake of salt and is known as one of the biomarkers for hypertension in the human body. Higher concentrations of sodium lead to increased activity of the ENaC protein in sodium absorption. In this study, a self-made immunosensor was developed using a homemade Printed Circuit Board-Screen Printed Carbon Electrode (PCB-SPCE) modified with cerium oxide. Anti-ENaC was immobilized on the surface of PCB-SPCE/ceria at pH 7.4, relying on the interaction between carboxyl groups of anti-ENaC and cerium oxide to detect the ENaC protein. Additionally, a portable in-house potentiostat named “UnpadStat” was developed for integration with the immunosensor. UnpadStat features a 5-in. touch screen display to showcase measurement data. Cyclic voltammetry measurements using the redox system of K3[Fe(CN)6] were applied to bare PCB-SPCE, PCB-SPCE/Ceria, PCB-SPCE/Ceria/Anti-ENaC, and PCB-SPCE/Ceria/Anti-ENaC/ENaC. Measurement results indicated an increase in current after modification with cerium, reaching 73.805 µA compared to unmodified (63.256 µA). After anti-ENaC immobilization, there was a decrease in current to 64.456 µA, and upon binding with the ENaC protein, a further decrease in current occurred, corresponding to the concentration of the ENaC protein. The detection limit obtained in this study was 0.133 ng/mL, and the quantification limit was 0.444 ng/mL for the concentration range of ENaC protein from 0.375 ng/mL to 6.0 ng/mL. The integration of the PCB-based immunosensor and UnpadStat can be utilized to determine the levels of ENaC protein in non-hypertensive urine samples and hypertensive patients.

Electrochemical detection of benzenediols using carbon-supported catalysts

A novel implementation of an electrochemical sensors making use of Screen-Printed Electrodes (SPE) has been discussed. SPE's modified with Carbon-supported Platinum (Pt/C) and Gold (Au/C) were used to detect the three benzenediol isomers, Catechol (CC), Hydroquinone (HQ) and Resorcinol (RS) in acidic media using traditional electrochemical analytical methods such as Cyclic Voltammetry (CV), Chronoamperometry (CA) and Differential Pulse Voltammetry (DPV). Detection of each benzenediol in isolation was possible by CV measurements, and peak oxidation potentials for each isomer were noted. Simultaneous detection of more than one, or all analytes in the same solution was also observed through DPV, once again noting the peak oxidation potentials. Quantification limits were observed using CA's across concentration values ranging from close to saturation down to 1 mM for CC and HQ, and 100 nM for RS, until the recorded current values were nearly indistinguishable to a blank 1 M HCl solution containing no analyte(s), and also evaluating the maximum possible linear range of sensing. The analytes were introduced to the sensor elements in controlled amounts and the electrochemical responses of the sensor elements were recorded and processed. Measurements were repeated across two potentiostats to ensure reproducibility. With these results, successful detection of benzenediols in acidic environment was possible using modified SPE's, proving a potential viable mechanism for quick, simple and inexpensive Volatile Toxic Organic Compounds (VTOC) detection and monitoring.

Experimental and computational study on antioxidant activity and molecular properties of novel ferrocenyl Schiff bases

In this study, antioxidant and molecular properties of some important novel ferrocenyl Schiff bases were studied. The 4-Ferrocenyl aniline synthetic pathway was chosen as the general procedure for the synthesis of Schiff bases. Two experimental techniques, UV–Visible spectroscopy and cyclic voltammetry, and one theoretical DFT method was employed to find out their antioxidant activity and molecular properties of some novel ferrocenyl Schiff bases and compared it with standard antioxidant (Ascorbic acid). Maximum wavelength, extinction coefficient, IC30 and IC50 were estimated by using UV–Visible spectroscopy. For theoretical investigations, computational Amsterdam density function software was employed to study the molecular properties and reaction parameters based on density functional theory calculations. The cyclic voltammetry (CV) measurements in electrochemical experiments were done at room temperature while diffusion coefficient was estimated by using CV graphs. UV–Vis spectra of these compounds exhibited similar peaks with greater intensity ranges from 312 nm to 314 nm and smaller intensity ranges 471 nm to 473 nm which occurred because of the only substituent R (naphthoxy, phenoxy and phenoxy) in these compounds. Registered Amsterdam density function was utilized to determine the optimized structure, FTIR spectra, UV–Visible spectra, HOMO, LUMO, dipole moment, ionization potential, electron affinity, band gap, hardness, chemical potential and electrophility index. The overall electrode processes were found to be diffusion controlled and the novel compounds showed appreciable antioxidant activities.