All-Carbon Electrode Consisting of Carbon Nanotubes on Graphite Foil for Flexible Electrochemical Applications

We demonstrate the fabrication of an all-carbon electrode by plasma-enhanced chemical vapor deposition for use in flexible electrochemical applications. The electrode is composed of vertically aligned carbon nanotubes that are grown directly on a flexible graphite foil. Being all-carbon, the simple fabrication process and the excellent electrochemical characteristics present an approach through which high-performance, highly-stable and cost-effective electrochemical applications can be achieved.     

Effect of the Preparation Conditions on the Catalytic Properties of CoPt for Highly Efficient 4-Nitrophenol Reduction

CoPt alloys with Pt contents from 15 to 90% were prepared using low-cost electrochemical deposition. Different samples were synthesized from electrochemical baths at pH = 2.5 and 5.5 in a solution with and without saccharin as an additive. The morphology, composition and crystalline structure of the as-prepared samples were investigated by High Resolution—Scanning Electron Microscopy (HR-SEM), Atomic Force Microscopy (AFM), Ultra-high Resolution—Transmission Electron Microscopy (UHR-TEM), Energy-Dispersive X-ray Spectroscopy (EDX), and X-ray Diffraction (XRD). XRD investigations revealed that fcc crystalline structure transforms into hcp crystalline structure when the pH of the electrochemical bath is increased from 2.5 to 5.5 as well as when saccharin is added to the electrochemical bath. The catalytic performance of the CoPt alloys for the nitro to amino phenol compounds conversion was investigated for all the prepared samples, and the results show that the conversion degree increases (from 11.4 to 96.5%) even though the Pt content in the samples decreases. From the samples prepared from the electrochemical bath with saccharin, a study regarding the effect of contact time was performed. The results indicated that after only 5 min, the CoPt sample prepared at pH = 5.5 in the presence of saccharin completely converted the nitro compound to an amino compound.     

Effect of Sintering Temperature on Adhesion Property and Electrochemical Activity of Pt/YSZ Electrode

The (Pt/YSZ)/YSZ sensor unit is the basic component of the NO_x sensor, which can detect the emission of nitrogen oxides in exhaust fumes and optimize the fuel combustion process. In this work, the effect of sintering temperature on adhesion property and electrochemical activity of Pt/YSZ electrode was investigated. Pt/YSZ electrodes were prepared at different sintering temperatures. The microstructure of the Pt/YSZ electrodes, as well as the interface between Pt/YSZ electrode and YSZ electrolyte, were observed by SEM. Chronoamperometry, linear scan voltammetry, and AC impedance were tested by the electrochemical workstation. The results show that increasing the sintering temperature (≤1500 °C) helped to improve adhesion property and electrochemical activity of the Pt/YSZ electrode, which benefited from the formation of the porous structure of the Pt/YSZ electrode. For the (Pt/YSZ) electrode/YSZ electrolyte system, O²⁻ in YSZ is converted into chemisorbed O₂ on Pt/YSZ, which is desorbed into the gas phase in the form of molecular oxygen; this process could be the rate-controlling step of the anodic reaction. Increasing the sintering temperature (≤1500 °C) could reduce the reaction activation energy of the Pt/YSZ electrode. The activation energy reaches the minimum value (1.02 eV) when the sintering temperature is 1500 °C.     

Nanocarbon Type Xerogel Materials Designed for Water Desalination

The relative performance of different porous solids in different applications is highly dependent on the internal pore structure of each material. Highly porous carbon materials can be prepared by evaporative drying and the pyrolysis of resorcinol-formaldehyde gels. By determining the correct synthesis parameters, the pore system of such materials can be reshaped. Depending on some important processing factors such as the dilution ratio or the initial pH of the precursor solution, various porous or non-porous carbon materials can be synthesized. This paper addresses carbon xerogels (CX) designed as a material electrode in capacitive deionization (CDI) systems for water desalination. In this work CX materials were synthesized via poly-condensation reactions of resorcinol with formaldehyde (RF) on a carbon felt sheet followed by pyrolysis. The resulting sheets were used as electrodes to develop a CDI experimental multi-cell laboratory system. The initial pH of the RF solution and the dilution ratio effect on the resulting carbon surface area and structure were analyzed. Surface area measurements using the BET method and an electrochemical capacitance evaluation of the obtained xerogels through electrochemical impedance spectroscopy were also performed. Finally, using our experimental CDI multi-cell laboratory system based on the obtained CX, we discuss the experimental data for the desalination rate as a function of the voltage and salt concentration. As a result, the developed model’s efficiency is demonstrated. The main goal of this work was to develop an efficient electrode-based novel carbon that could be commercially competitive, as well as to create guidelines for future desalination research using CX electrode materials.     

Improvement in NO2 Gas Sensing Properties of Semiconductor-Type Sensors by Loading Pt into BiVO4 Nanocomposites at Room Temperature

In the present study, we report the first attempt to prepare a conducive environment for Pt/BiVO₄ nanocomposite material reusability for the promotion of sustainable development. Here, the Pt/BiVO₄ nanocomposite was prepared using a hydrothermal method with various weight percentages of platinum for use in NO₂ gas sensors. The surface morphologies and structure of the Pt/BiVO₄ nanocomposite were characterized by scanning electron microscope (SEM), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray diffraction (XRD). The results showed that Pt added to BiVO₄ with 3 wt.% Pt/BiVO₄ was best at a concentration of 100 ppm NO₂, with a response at 167.7, and a response/recovery time of 12/35 s, respectively. The Pt/BiVO₄ nanocomposite-based gas sensor exhibits promising nitrogen dioxide gas-sensing characteristics, such as fast response, highly selective detection, and extremely short response/recovery time. Additionally, the mechanisms of gas sensing in Pt/BiVO₄ nanocomposites were explored in this paper.     

Electrically Switchable Film Structure of Conjugated Polymer Composites

Domains rich in different blend components phase-separate during deposition, creating a film morphology that determines the performance of active layers in organic electronics. However, morphological control either relies on additional fabrication steps or is limited to a small region where an external interaction is applied. Here, we show that different semiconductor-insulator polymer composites can be rapidly dip-coated with the film structure electrically switched between distinct morphologies during deposition guided by the meniscus formed between the stationary barrier and horizontally drawn solid substrate. Reversible and repeatable changes between the morphologies used in devices, e.g., lateral morphologies and stratified layers of semiconductors and insulators, or between phase-inverted droplet-like structures are manifested only for one polarity of the voltage applied across the meniscus as a rectangular pulse. This phenomenon points to a novel mechanism, related to voltage-induced doping and the doping-dependent solubility of the conjugated polymer, equivalent to an increased semiconductor content that controls the composite morphologies. This is effective only for the positively polarized substrate rather than the barrier, as the former entrains the nearby lower part of the coating solution that forms the final composite film. The mechanism, applied to the pristine semiconductor solution, results in an increased semiconductor deposition and 40-times higher film conductance.     

Activation of Porous Pt Electrodes Deposited on YSZ Electrolyte by Nitric Acid Treatment

The effect of nitric acid treatment on the electrochemical performance of porous Pt electrodes deposited on YSZ (abbreviation from yttria stabilized zirconia) electrolyte was investigated. Two identical symmetrical Pt/YSZ/Pt cells with porous Pt electrodes were fabricated, after which the electrodes of the first cell were kept as sintered, while those of the second cell were impregnated with HNO₃ solution. The electrochemical behavior of the prepared electrodes was studied using impedance spectroscopy and cyclic voltammetry. Significant reduction of the polarization resistance of the HNO₃-treated electrodes was revealed. The observed enhancement of the electrochemical performance of porous Pt electrodes was assumed to be caused by adsorption of NO_x-species on YSZ and Pt surfaces, which promotes oxygen molecules dissociation and transport to the triple phase boundary by the “relay-race” mechanism. The obtained results allow for considering the nitric acid treatment of a porous Pt electrode as an effective way of electrode activation.     

Opportunities,Challenges and Prospects for Electrodeposition of Thin-Film Functional Layers in Solid Oxide Fuel Cell Technology

Electrolytic deposition (ELD) and electrophoretic deposition (EPD) are relevant methods for creating functional layers of solid oxide fuel cells (SOFCs). This review discusses challenges, new findings and prospects for the implementation of these methods, with the main emphasis placed on the use of the ELD method. Topical issues concerning the formation of highly active SOFC electrodes using ELD, namely, the electrochemical introduction of metal cations into a porous electrode backbone, the formation of composite electrodes, and the electrochemical synthesis of perovskite-like electrode materials are considered. The review presents examples of the ELD formation of the composite electrodes based on porous platinum and silver, which retain high catalytic activity when used in the low-temperature range (400–650 °C). The features of the ELD/EPD co-deposition in the creation of nanostructured electrode layers comprising metal cations, ceramic nanoparticles, and carbon nanotubes, and the use of EPD to create oriented structures are also discussed. A separate subsection is devoted to the electrodeposition of CeO₂-based film structures for barrier, protective and catalytic layers using cathodic and anodic ELD, as well as to the main research directions associated with the deposition of the SOFC electrolyte layers using the EPD method.     

Good Choice of Electrode Material as the Key to Creating Electrochemical Sensors—Characteristics of Carbon Materials and Transparent Conductive Oxides (TCO)

The search for new electrode materials has become one of the goals of modern electrochemistry. Obtaining electrodes with optimal properties gives a product with a wide application potential, both in analytics and various industries. The aim of this study was to select, from among the presented electrode materials (carbon and oxide), the one whose parameters will be optimal in the context of using them to create sensors. Electrochemical impedance spectroscopy and cyclic voltammetry techniques were used to determine the electrochemical properties of the materials. On the other hand, properties such as hydrophilicity/hydrophobicity and their topological structure were determined using contact angle measurements and confocal microscopy, respectively. Based on the research carried out on a wide group of electrode materials, it was found that transparent conductive oxides of the FTO (fluorine doped tin oxide) type exhibit optimal electrochemical parameters and offer great modification possibilities. These electrodes are characterized by a wide range of work and high chemical stability. In addition, the presence of a transparent oxide layer allows for the preservation of valuable optoelectronic properties. An important feature is also the high sensitivity of these electrodes compared to other tested materials. The combination of these properties made FTO electrodes selected for further research.     

Nanotube Functionalization: Investigation,Methods and Demonstrated Applications

This review presents an update on nanotube functionalization, including an investigation of their methods and applications. The review starts with the discussion of microscopy and spectroscopy investigations of functionalized carbon nanotubes (CNTs). The results of transmission electron microscopy and scanning tunnelling microscopy, X-ray photoelectron spectroscopy, infrared spectroscopy, Raman spectroscopy and resistivity measurements are summarized. The update on the methods of the functionalization of CNTs, such as covalent and non-covalent modification or the substitution of carbon atoms, is presented. The demonstrated applications of functionalized CNTs in nanoelectronics, composites, electrochemical energy storage, electrode materials, sensors and biomedicine are discussed.     

Preparation of Dispersed Platinum Nanoparticles on a Carbon Nanostructured Surface Using Supercritical Fluid Chemical Deposition

We have developed a method of forming platinum (Pt) nanoparticles using a metal organic chemical fluid deposition (MOCFD) process employing a supercritical fluid (SCF), and have demonstrated the synthesis of dispersed Pt nanoparticles on the surfaces of carbon nanowalls (CNWs), two-dimensional carbon nanostructures, and carbon nanotubes (CNTs). By using SCF-MOCFD with supercritical carbon dioxide as a solvent of metal-organic compounds, highly dispersed Pt nanoparticles of 2 nm diameter were deposited on the entire surface of CNWs and CNTs. The SCF-MOCFD process proved to be effective for the synthesis of Pt nanoparticles on the entire surface of intricate carbon nanostructures with narrow interspaces.     

Effects of Fe Impurities on Self-Discharge Performance of Carbon-Based Supercapacitors

Activated carbon is widely used as an electrode material in supercapacitors due to its superior electrochemical stability, excellent electrical conductivity, and environmental friendliness. In this study, the self-discharge mechanisms of activated carbon electrodes loaded with different contents of Fe impurities (Fe and Fe₃O₄) were analyzed by multi-stage fitting to explore the tunability of self-discharge. It is was found that a small quantity of Fe impurities on carbon materials improves the self-discharge performance dominated by redox reaction, by adjusting the surface state and pore structure of carbon materials. As the content of Fe impurities increases, the voltage loss of activated carbon with the Fe impurity concentrations of 1.12 wt.% (AF-1.12) decreases by 37.9% of the original, which is attributable to the reduce of ohmic leakage and diffusion, and the increase in Faradic redox at the electrode/electrolyte interface. In summary, self-discharge performance of carbon-based supercapacitors can be adjusted via the surface state and pour structure, which provides insights for the future design of energy storage.     

Non-enzymatic Hydrogen Peroxide Sensors Based on Multi-wall Carbon Nanotube/Pt Nanoparticle Nanohybrids

A novel strategy to fabricate a hydrogen peroxide (H₂O₂) sensor was developed by using platinum (Pt) electrodes modified with multi-wall carbon nanotube-platinum nanoparticle nanohybrids (MWCNTs/Pt nanohybrids). The process to synthesize MWCNTs/Pt nanohybrids was simple and effective. Pt nanoparticles (Pt NPs) were generated in situ in a potassium chloroplatinate aqueous solution in the presence of multi-wall carbon nanotubes (MWCNTs), and readily attached to the MWCNTs convex surfaces without any additional reducing reagents or irradiation treatment. The MWCNT/Pt nanohybrids were characterized by transmission electron microscope (TEM), and the redox properties of MWCNTs/Pt nanohybrids-modified Pt electrode were studied by electrochemical measurements. The MWCNTs/Pt-modified electrodes exhibited a favorable catalytic ability in the reduction of H₂O₂. The modified electrodes can be used to detect H₂O₂ in the range of 0.01–2 mM with a lower detection limit of 0.3 μM at a signal-to-noise ratio of 3. The sensitivity of the electrode to H₂O₂ was calculated to be 205.80 μA mM⁻¹ cm⁻² at working potential of 0 mV. In addition, the electrodes exhibited an excellent reusability and long-term stability as well as negligible interference from ascorbic acid, uric acid, and acetaminophen.     

Designing Spinel Li4Ti5O12 Electrode as Anode Material for Poly(ethylene)oxide-Based Solid-State Batteries

The development of a promising Li metal solid-state battery (SSB) is currently hindered by the instability of Li metal during electrodeposition; which is the main cause of dendrite growth and cell failure at elevated currents. The replacement of Li metal anode by spinel Li₄Ti₅O₁₂ (LTO) in SSBs would avoid such problems, endowing the battery with its excellent features such as long cycling performance, high safety and easy fabrication. In the present work, we provide an evaluation of the electrochemical properties of poly(ethylene)oxide (PEO)-based solid-state batteries using LTO as the active material. Electrode laminates have been developed and optimized using electronic conductive additives with different morphologies such as carbon black and multiwalled carbon nanotubes. The electrochemical performance of the electrodes was assessed on half-cells using a PEO-based solid electrolyte and a lithium metal anode. The optimized electrodes displayed an enhanced capability rate, delivering 150 mAh g⁻¹ at C/2, and a stable lifespan over 140 cycles at C/20 with a capacity retention of 83%. Moreover, postmortem characterization did not evidence any morphological degradation of the components after ageing, highlighting the long-cycling feature of the LTO electrodes. The present results bring out the opportunity to build high-performance solid-state batteries using LTO as anode material.     

Removal of Thiol-SAM on a Gold Surface for Re-Use of an Interdigitated Chain-Shaped Electrode

The self-assembled monolayer (SAM) is the most common organic assembly utilized for the formation of the monolayers of alkane-thiolates on gold electrode, resulting in a wide range of applications for the modified SAM on gold in various research areas. This study examined the desorption of a SAM that was developed on the gold surface of an interdigitated chain-shaped electrode (the ICE, a unique electrode design, was fabricated by our group) with the goal of determining the most efficient strategy of SAM removal for the ICE to be re-used. A simple and proficient solution-based cleaning procedure was applied for the removal of a SAM on the gold surface of the ICE by using a sodium borohydride solution within short-term treatment, resulting in efficiency for the recovery of the originally electrochemical characteristic of ICE of 90.3%. The re-use of ICE after the removal process was confirmed by the successful re-deposition of a SAM onto the electrode surface, resulting in the high efficiency percentage of 90.1% for the reusability of ICE with the SAM modification. Electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV) were used as tools to investigate the changes in the electrode interface at each stage of the SAM removal and the electrode recycling. X-ray photoelectron spectroscopy and Fourier-transform infrared spectroscopy were employed, being powerful spectrum techniques, for the characterization of the bonding structure and chemical state of the bare ICE and the modified ICE at each treatment step. Based on the comprehensive discussion of analytical chemistry from the obtained EIS and CV data in this study, we confirmed and proved the effectiveness of this promising method for the removal of a SAM from the ICE and the re-use of ICE in the field of material deposition, with the aims of saving money, improving experimental handling, and protecting the environment.     

Electroless Platinum Deposition Using Co3+/Co2+ Redox Couple as a Reducing Agent

In the present work, the kinetics of electroless deposition of Pt, using a cobalt ion redox system (Co³⁺/Co²⁺) as a reducing agent, has been investigated. The deposition rate of Pt depends on the pH, concentration of reactants, and temperature. The deaeration and bubbling of the plating solution with argon play an essential role. It was found that 0.11 mg cm⁻² of Pt films could be deposited on the surface of a roughed glass sheet in one hour without replenishing the solution. Additional data have been obtained on the grounds of electrochemical quartz crystal microbalance experiments. The bubbling (agitation) of the electroless Pt plating solution with argon during the deposition of Pt results in a higher deposition rate and is ca. 3 µg cm⁻² min⁻¹. The Pt deposition rate is far less, and is as low as 0.14 µg cm⁻² min⁻¹ when the electroless Pt plating solution is not bubbled with argon during the deposition of Pt.     

Facile Synthesis of Carbon Nanospheres with High Capability to Inhale Selenium Powder for Electrochemical Energy Storage

Carbon–selenium composite positive electrode (CSs@Se) is engineered in this project using a melt diffusion approach with glucose as a precursor, and it demonstrates good electrochemical performance for lithium–selenium batteries. X-ray diffraction (XRD) and scanning electron microscopy (SEM) with EDS analysis are used to characterize the newly designed CSs@Se electrode. To complete the evaluation, electrochemical characterization such as charge–discharge (rate performance and cycle stability), cyclic voltammetry (CV), and electrochemical impedance spectroscopy (EIS) tests are done. The findings show that selenium particles are distributed uniformly in mono-sized carbon spheres with enormous surface areas. Furthermore, the charge–discharge test demonstrates that the CSs@Se cathode has a rate performance of 104 mA h g⁻¹ even at current density of 2500 mA g⁻¹ and can sustain stable cycling for 70 cycles with a specific capacity of 270 mA h g⁻¹ at current density of 25 mA g⁻¹. The homogeneous diffusion of selenium particles in the produced spheres is credited with an improved electrochemical performance.     

Electrode Design for MnO2-Based Aqueous Electrochemical Capacitors: Influence of Porosity and Mass Loading

The purpose of this study is to highlight the influence of some fabrication parameters, such as mass loading and porosity, which are not really elucidated and standardized during the realization of electrodes for supercapacitors, especially when using metal oxides as electrode materials. Electrode calendering, as one stage during the fabrication of electrodes, was carried out step-by-step on manganese dioxide electrodes to study the decreasing porosity effect on the electrochemical performance of a MnO₂ symmetric device. One other crucial parameter, the mass loading, which has to be understood and well used for realistic supercapacitors, was investigated concurrently. Gravimetric, areal and volumetric capacitances are highlighted, varying the porosity for low-, medium- and large-mass loading. Low-loading leads to the best specific capacitances but is not credible for realistic supercapacitors, except for microdevices. Down 50% porosities after calendering, capacitances are increased and become stable faster, suggesting a faster wettability of the dense electrodes by the electrolyte, especially for high-mass loading. EIS experiments performed on electrodes without and with calendering lead to a significant decrease of the device’s time response, especially at high loading. A high-mass loading device seems to work as a power battery, whereas electrode calendaring, which allows decreasing the time response, leads to an electrical behavior closer to that expected for a supercapacitor.