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A special issue of Nanomaterials (ISSN 2079-4991). This special issue belongs to the section "Energy and Catalysis".

Deadline for manuscript submissions: closed (30 April 2023) | Viewed by 36338

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Prof. Dr. Domenica Tonelli

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Department Industrial Chemistry "Toso Montanari", University of Bologna, Viale Risorgimento 4, 40136 Bologna, Italy
Interests: analytical chemistry; sensors; biosensors; materials characterization; food analysis; environmental analysis; electrochemical devices; chemically modified electrodes; layered double hydroxides; conducting polymers; electrosynthesis; nanomaterials; metal nanoparticles; nanocomposites; energy storage; energy conversion
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Dr. Isacco Gualandi

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Department of Industrial Chemistry "Toso Montanari", University of Bologna, Viale Risorgimento 4, 40136 Bologna, Italy
Interests: materials chemistry; analytical chemistry; electrochemistry; organic transistors; nanostructured materials; electrochemical sensors
Special Issues, Collections and Topics in MDPI journals

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Dear Colleagues,

Electrochemical devices are attracting major attention in the fields of sensing, batteries, supercapacitors, water splitting reaction, CO₂reduction, fuel cells, electrocatalysis, and ecc. The direct conversion of chemical into electrical energy represents a smart solution in the field of energy storage and conversion. On the other hand, the direct acquisition of an electrical signal stemming from an analyte presence represents a quick and simple method for the development of a sensor. Nanomaterials are a powerful tool to boost performances of electrochemical devices due to their high surface/volume ratio, surface reactivity, and improved accessibility.

In this Special Issue, we welcome research papers and reviews focusing on the recent applications, synthesis, and characterization of nanomaterials for electrochemistry, as well as cutting-edge technological strategies for their use in real life. We would like to discuss the challenges that their development will bring. Long-term stability, low cost, and high efficiency should be obtained to attain a high technology readiness level for commercialization and to achieve a real impact on every-day life.

Prof. Dr. Domenica Tonelli
Dr. Isacco Gualandi
Guest Editors

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Keywords

electrochemistry
sensors
electrocatalysis
energy storage
supercapacitors
batteries
nanoparticles
carbon nanomaterials

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Published Papers (12 papers)

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Research

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16 pages, 7477 KiB

Open AccessArticle

The Influence of TiO₂ Nanoparticles Morphologies on the Performance of Lithium-Ion Batteries

by Wenpo Luo, Juliette Blanchard, Yanpeng Xue and Abdelhafed Taleb

Nanomaterials 2023, 13(19), 2636; https://doi.org/10.3390/nano13192636 - 25 Sep 2023

Cited by 2 | Viewed by 1273

Abstract

Anode materials based on the TiO₂ nanoparticles of different morphologies were prepared using the hydrothermal method and characterized by various techniques, such as X-ray diffraction (XRD), field-emission scanning electron microscopy (FE-SEM), and N₂ absorption. The TiO₂ nanoparticles prepared were used as anode materials for lithium-ion batteries (LIBs), and their electrochemical properties were tested using discharging/charging measurements. The results showed that the initial morphology of the nanoparticles plays a minor role in battery performance after the first few cycles and that better capacity was achieved for TiO₂ nanobelt morphology. The sharp drop in the specific capacity of LIB during their first cycles is examined by considering changes in the morphology of TiO₂ particles and their porosity properties in terms of size and connectivity. The performance of TiO₂ anode materials has also been assessed by considering their phase. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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13 pages, 2272 KiB

Open AccessArticle

The Influence of Electrode Thickness on the Structure and Water Splitting Performance of Iridium Oxide Nanostructured Films

by Abeer S. Altowyan, Mohamed Shaban, Khaled Abdelkarem and Adel M. El Sayed

Nanomaterials 2022, 12(19), 3272; https://doi.org/10.3390/nano12193272 - 21 Sep 2022

Cited by 11 | Viewed by 2321

Abstract

For a safe environment, humanity should be oriented towards renewable energy technology. Water splitting (WS), utilizing a photoelectrode with suitable thickness, morphology, and conductivity, is essential for efficient hydrogen production. In this report, iridium oxide (IrO_x) films of high conductivity were spin-cast on glass substrates. FE-SEM showed that the films are of nanorod morphology and different thicknesses. UV-Vis spectra indicated that the absorption and reflectance of the films depend on their thickness. The optical band gap (E_g) was increased from 2.925 eV to 3.07 eV by varying the spin speed (SS) of the substrates in a range of 1.5 × 10³–4.5 × 10³ rpm. It was clear from the micro-Raman spectra that the films were amorphous. The E_g vibrational mode of Ir–O stretching was red-shifted from 563 cm⁻¹ (for the rutile IrO₂ single crystal) to 553 cm⁻¹. The IrO_x films were used to develop photoelectrochemical (PEC) hydrogen production catalysts in 0.5M of sodium sulfite heptahydrate Na₂SO₃·7H₂O (2-electrode system), which exhibits higher hydrogen evaluation (HE) reaction activity, which is proportional to the thickness and absorbance of the used IrO_x photocathode, as it showed an incident photon-to-current efficiency (IPCE%) of 7.069% at 390 nm and −1 V. Photocurrent density (Jph = 2.38 mA/cm² at −1 V vs. platinum) and PEC hydrogen generation rate (83.68 mmol/ h cm² at 1 V) are the best characteristics of the best electrode (the thickest and most absorbent IrO_x photocathode). At −1 V and 500 nm, the absorbed photon-to-current conversion efficiency (APCE%) was 7.84%. Electrode stability, thermodynamic factors, solar-to-hydrogen conversion efficiency (STH), and electrochemical impedance spectroscopies (EISs) were also studied. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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23 pages, 5620 KiB

Open AccessFeature PaperArticle

Nanoparticles of Mixed-Valence Oxides Mn_XCO_3-XO₄ (0 ≤ X ≤ 1) Obtained with Agar-Agar from Red Algae (Rhodophyta) for Oxygen Evolution Reaction

by Jakeline Raiane D. Santos, Rafael A. Raimundo, Thayse R. Silva, Vinícius D. Silva, Daniel A. Macedo, Francisco J. A. Loureiro, Marco A. M. Torres, Domenica Tonelli and Uílame U. Gomes

Nanomaterials 2022, 12(18), 3170; https://doi.org/10.3390/nano12183170 - 13 Sep 2022

Cited by 5 | Viewed by 1989

Abstract

The development of efficient electrocatalysts for the oxygen evolution reaction (OER) is of paramount importance in sustainable water-splitting technology for hydrogen production. In this context, this work reports mixed-valence oxide samples of the Mn_XCo_3-XO₄ type (0 ≤ X ≤ 1) synthesized for the first time by the proteic sol-gel method using Agar-Agar as a polymerizing agent. The powders were calcined at 1173 K, characterized by FESEM, XRD, RAMAN, UV–Vis, FT-IR, VSM, and XPS analyses, and were investigated as electrocatalysts for the oxygen evolution reaction (OER). Through XRD analysis, it was observed that the pure cubic phase was obtained for all samples. The presence of Co³⁺, Co²⁺, Mn²⁺, Mn³⁺, and Mn⁴⁺ was confirmed by X-ray spectroscopy (XPS). Regarding the magnetic measurements, a paramagnetic behavior at 300 K was observed for all samples. As far as OER is concerned, it was investigated in an alkaline medium, where the best overpotential of 299 mV vs. RHE was observed for the sample (MnCo₂O₄), which is a lower value than those of noble metal electrocatalysts in the literature, together with a Tafel slope of 52 mV dec⁻¹, and excellent electrochemical stability for 15 h. Therefore, the green synthesis method presented in this work showed great potential for obtaining electrocatalysts used in the oxygen evolution reaction for water splitting. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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12 pages, 2050 KiB

Open AccessArticle

Poly(Thiophene)/Graphene Oxide-Modified Electrodes for Amperometric Glucose Biosensing

by Maria I. Pilo, Sylwia Baluta, Anna C. Loria, Gavino Sanna and Nadia Spano

Nanomaterials 2022, 12(16), 2840; https://doi.org/10.3390/nano12162840 - 18 Aug 2022

Cited by 5 | Viewed by 1908

Abstract

The availability of fast and non-expensive analytical methods for the determination of widespread interest analytes such as glucose is an object of large relevance; this is so not only in the field of analytical chemistry, but also in medicinal and in food chemistry. In this context, electrochemical biosensors have been proposed in different arrangements, according to the mode of electron transfer between the bioreceptor and the electrode. An efficient immobilization of an enzyme on the electrode surface is essential to assure satisfactory analytical performances of the biosensor in terms of sensitivity, limit of detection, selectivity, and linear range of employment. Here, we report the use of a thiophene monomer, (2,5-di(2-thienyl)thieno [3,2-b]thiophene (dTT-bT), as a precursor of an electrogenerated conducting film to immobilize the glucose oxidase (GOx) enzyme on Pt, glassy carbon (GC), and Au electrode surfaces. In addition, the polymer film electrochemically synthetized on a glassy carbon electrode was modified with graphene oxide before the deposition of GOx; the analytical performances of both the arrangements (without and with graphene oxide) in the glucose detection were compared. The biosensor containing graphene oxide showed satisfactory values of linear dynamic range (1.0–10 mM), limit of detection (0.036 mM), and sensitivity (9.4 µA mM⁻¹ cm⁻²). Finally, it was tested in the determination of glucose in fruit juices; the interference from fructose, saccharose, and ascorbic acid was evaluated. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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11 pages, 5316 KiB

Open AccessArticle

An Effective Label-Free Electrochemical Aptasensor Based on Gold Nanoparticles for Gluten Detection

by Rossella Svigelj, Ivan Zuliani, Cristian Grazioli, Nicolò Dossi and Rosanna Toniolo

Nanomaterials 2022, 12(6), 987; https://doi.org/10.3390/nano12060987 - 17 Mar 2022

Cited by 22 | Viewed by 4033

Abstract

Nanomaterials can be used to modify electrodes and improve the conductivity and the performance of electrochemical sensors. Among various nanomaterials, gold-based nanostructures have been used as an anchoring platform for the functionalization of biosensor surfaces. One of the main advantages of using gold for the modification of electrodes is its great affinity for thiol-containing molecules, such as proteins, forming a strong Au-S bond. In this work, we present an impedimetric biosensor based on gold nanoparticles and a truncated aptamer for the quantification of gluten in hydrolyzed matrices such as beer and soy sauce. A good relationship between the R_ct values and PWG-Gliadin concentration was found in the range between 0.1–1 mg L⁻¹ of gliadin (corresponding to 0.2–2 mg L⁻¹ of gluten) with a limit of detection of 0.05 mg L⁻¹ of gliadin (corresponding to 0.1 mg L⁻¹ of gluten). The label-free assay was also successfully applied for the determination of real food samples. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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14 pages, 2482 KiB

Open AccessArticle

Electrochemical and X-ray Photoelectron Spectroscopy Surface Characterization of Interchain-Driven Self-Assembled Monolayer (SAM) Reorganization

by Angelo Tricase, Anna Imbriano, Nicoletta Ditaranto, Eleonora Macchia, Rosaria Anna Picca, Davide Blasi, Luisa Torsi and Paolo Bollella

Nanomaterials 2022, 12(5), 867; https://doi.org/10.3390/nano12050867 - 4 Mar 2022

Cited by 4 | Viewed by 2521

Abstract

Herein, we report a combined strategy encompassing electrochemical and X-ray photoelectron spectroscopy (XPS) experiments to investigate self-assembled monolayer (SAM) conformational reorganization onto an electrode surface due to the application of an electrical field. In particular, 3-mercaptopriopionic acid SAM (3MPA SAM) modified gold electrodes are activated with a 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide (EDC) and N-hydroxysulfosuccinimide (NHSS) (EDC-NHSS) mixture by shortening the activation time, from 2 h to 15/20 min, labelled as Protocol-A, -B and -C, respectively. This step, later followed by a deactivation process with ethanolamine (EA), plays a key role in the reaction yields (formation of N-(2-hydroxyethyl)-3-mercaptopropanamide, NMPA) but also in the conformational rearrangement observed during the application of the electrical field. This study aims at explaining the high performance (i.e., single-molecule detection at a large electrode interface) of bioelectronic devices, where the 3MPA-based SAM structure is pivotal in achieving extremely high sensing performance levels due to its interchain interaction. Cyclic voltammetry (CV) experiments performed in K₄Fe(CN)₆:K₃Fe(CN)₆ for 3MPA SAMs that are activated/deactivated show similar trends of anodic peak current (I_A) over time, mainly related to the presence of interchain hydrogen bonds, driving the conformational rearrangements (tightening of SAMs structure) while applying an electrical field. In addition, XPS analysis allows correlation of the deactivation yield with electrochemical data (conformational rearrangements), identifying the best protocol in terms of high reaction yield, mainly related to the shorter reaction time, and not triggering any side reactions. Finally, Protocol-C’s SAM surface coverage, determined by CV in H₂SO₄ and differential pulse voltammetry (DPV) in NaOH, was 1.29 * 10¹³ molecules cm⁻², being similar to the bioreceptor surface coverage in single-molecule detection at a large electrode interface. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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20 pages, 8283 KiB

Open AccessArticle

Synthesis and Characterization of NiCoPt/CNFs Nanoparticles as an Effective Electrocatalyst for Energy Applications

by Esam E. Abdel-Hady, Mohamed Shaban, Mohamed O. Abdel-Hamed, Ahmed Gamal, Heba Yehia and Ashour M. Ahmed

Nanomaterials 2022, 12(3), 492; https://doi.org/10.3390/nano12030492 - 30 Jan 2022

Cited by 16 | Viewed by 2805

Abstract

In this work, three nanoparticle samples, Ni₄Co₂Pt/CNFs, Ni₅CoPt/CNFs and Ni₆Pt/CNFs, were designed according to the molar ratio during loading on carbon nanofibers (CNFs) using electrospinning and carbonization at 900 °C for 7 h in an argon atmosphere. The metal loading and carbon ratio were fixed at 20 and 80 wt%, respectively. Various analysis tools were used to investigate the chemical composition, structural, morphological, and electrochemical (EC) properties. For samples with varying Co%, the carbonization process reduces the fiber diameter of the obtained electrospun nanofibers from 200–580 nm to 150–200 nm. The EDX mapping revealed that nickel, platinum, and cobalt were evenly and uniformly incorporated into the carbonized PVANFs. The prepared Ni-Co-Pt/CNFs have a face-centered cubic (FCC) structure with slightly increased crystallite size as the Co% decreased. The electrocatalytic properties of the samples were investigated for ethanol, methanol and urea electrooxidation. Using cyclic voltammetry (CV), chronoamperometry, and electrochemical impedance measurements, the catalytic performance and electrode stability were investigated as a function of electrolyte concentration, scan rate, and reaction time. When Co is added to Ni, the activation energy required for the electrooxidation reaction decreases and the electrode stability increases. In 1.5 M methanol, the Ni₅CoPt/CNFs electrode showed the lowest onset potential and the highest current density (30.6 A/g). This current density is reduced to 28.2 and 21.2 A/g for 1.5 M ethanol and 0.33 M urea, respectively. The electrooxidation of ethanol, methanol, and urea using our electrocatalysts is a combination of kinetic/diffusion control limiting reactions. This research provided a unique approach to developing an efficient Ni-Co-Pt-based electrooxidation catalyst for ethanol, methanol and urea. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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19 pages, 4982 KiB

Open AccessArticle

Recycling Rusty Iron with Natural Zeolite Heulandite to Create a Unique Nanocatalyst for Green Hydrogen Production

by Mohamed Shaban, Mohammad BinSabt, Ashour M. Ahmed and Fatma Mohamed

Nanomaterials 2021, 11(12), 3445; https://doi.org/10.3390/nano11123445 - 20 Dec 2021

Cited by 8 | Viewed by 3600

Abstract

Corrosion-induced iron rust causes severe danger, pollution, and economic problems. In this work, nanopowders of Fe₂O₃ and Fe₂O₃/zeolite are synthesized for the first time using rusted iron waste and natural zeolite heulandite by chemical precipitation. The chemical composition, nanomorphologies, structural parameters, and optical behaviors are investigated using different techniques. The Fe₂O₃/zeolite nanocomposite showed smaller sizes and greater light absorption capability in visible light than Fe₂O₃ nanopowder. The XRD pattern shows crystalline hematite (α-Fe₂O₃) with a rhombohedral structure. The crystallite sizes for the plane (104) of the Fe₂O₃ and Fe₂O₃/zeolite are 64.84 and 56.53 nm, respectively. The Fe₂O₃ and Fe₂O₃/zeolite have indirect bandgap values of 1.87 and 1.91 eV and direct bandgap values of 2.04 and 2.07 eV, respectively. Fe₂O₃ and Fe₂O₃/zeolite nanophotocatalysts are used for solar photoelectrochemical (PEC) hydrogen production. The Fe₂O₃/zeolite exhibits a PEC catalytic hydrogen production rate of 154.45 mmol/g.h @ 1 V in 0.9 M KOH solution, which is the highest value yet for Fe₂O₃-based photocatalysts. The photocurrent density of Fe₂O₃/zeolite is almost two times that of Fe₂O₃ catalyst, and the IPCE (incident photon-to-current conversion efficiency) reached ~27.34%@307 nm and 1 V. The electrochemical surface area (ECSA) values for Fe₂O₃ and Fe₂O₃/zeolite photocatalysts were 7.414 and 21.236 m²/g, respectively. The rate of hydrogen production for Fe₂O₃/zeolite was 154.44 mmol h⁻¹/g. This nanophotocatalyst has a very low PEC corrosion rate of 7.6 pm/year; it can retain ~97% of its initial performance. Therefore, the present research can be applied industrially as a cost-effective technique to address two issues at once by producing solar hydrogen fuel and recycling the rusted iron wires. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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21 pages, 5152 KiB

Open AccessReview

Print-Light-Synthesis for Single-Step Metal Nanoparticle Synthesis and Patterned Electrode Production

by Stefano Gianvittorio, Domenica Tonelli and Andreas Lesch

Nanomaterials 2023, 13(13), 1915; https://doi.org/10.3390/nano13131915 - 23 Jun 2023

Cited by 1 | Viewed by 1820

Abstract

The fabrication of thin-film electrodes, which contain metal nanoparticles and nanostructures for applications in electrochemical sensing as well as energy conversion and storage, is often based on multi-step procedures that include two main passages: (i) the synthesis and purification of nanomaterials and (ii) the fabrication of thin films by coating electrode supports with these nanomaterials. The patterning and miniaturization of thin film electrodes generally require masks or advanced patterning instrumentation. In recent years, various approaches have been presented to integrate the spatially resolved deposition of metal precursor solutions and the rapid conversion of the precursors into metal nanoparticles. To achieve the latter, high intensity light irradiation has, in particular, become suitable as it enables the photochemical, photocatalytical, and photothermal conversion of the precursors during or slightly after the precursor deposition. The conversion of the metal precursors directly on the target substrates can make the use of capping and stabilizing agents obsolete. This review focuses on hybrid platforms that comprise digital metal precursor ink printing and high intensity light irradiation for inducing metal precursor conversions into patterned metal and alloy nanoparticles. The combination of the two methods has recently been named Print-Light-Synthesis by a group of collaborators and is characterized by its sustainability in terms of low material consumption, low material waste, and reduced synthesis steps. It provides high control of precursor loading and light irradiation, both affecting and improving the fabrication of thin film electrodes. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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35 pages, 3892 KiB

Open AccessReview

Focus Review on Nanomaterial-Based Electrochemical Sensing of Glucose for Health Applications

by Domenica Tonelli, Isacco Gualandi, Erika Scavetta and Federica Mariani

Nanomaterials 2023, 13(12), 1883; https://doi.org/10.3390/nano13121883 - 19 Jun 2023

Cited by 9 | Viewed by 2448

Abstract

Diabetes management can be considered the first paradigm of modern personalized medicine. An overview of the most relevant advancements in glucose sensing achieved in the last 5 years is presented. In particular, devices exploiting both consolidated and innovative electrochemical sensing strategies, based on nanomaterials, have been described, taking into account their performances, advantages and limitations, when applied for the glucose analysis in blood and serum samples, urine, as well as in less conventional biological fluids. The routine measurement is still largely based on the finger-pricking method, which is usually considered unpleasant. In alternative, glucose continuous monitoring relies on electrochemical sensing in the interstitial fluid, using implanted electrodes. Due to the invasive nature of such devices, further investigations have been carried out in order to develop less invasive sensors that can operate in sweat, tears or wound exudates. Thanks to their unique features, nanomaterials have been successfully applied for the development of both enzymatic and non-enzymatic glucose sensors, which are compliant with the specific needs of the most advanced applications, such as flexible and deformable systems capable of conforming to skin or eyes, in order to produce reliable medical devices operating at the point of care. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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33 pages, 8576 KiB

Open AccessReview

Recent Advances in Porous Carbon Materials as Electrodes for Supercapacitors

by Zhengdao Pan, Sheng Yu, Linfang Wang, Chenyu Li, Fei Meng, Nan Wang, Shouxin Zhou, Ye Xiong, Zhoulu Wang, Yutong Wu, Xiang Liu, Baizeng Fang and Yi Zhang

Nanomaterials 2023, 13(11), 1744; https://doi.org/10.3390/nano13111744 - 26 May 2023

Cited by 35 | Viewed by 5011

Abstract

Porous carbon materials have demonstrated exceptional performance in various energy and environment-related applications. Recently, research on supercapacitors has been steadily increasing, and porous carbon materials have emerged as the most significant electrode material for supercapacitors. Nonetheless, the high cost and potential for environmental pollution associated with the preparation process of porous carbon materials remain significant issues. This paper presents an overview of common methods for preparing porous carbon materials, including the carbon-activation method, hard-templating method, soft-templating method, sacrificial-templating method, and self-templating method. Additionally, we also review several emerging methods for the preparation of porous carbon materials, such as copolymer pyrolysis, carbohydrate self-activation, and laser scribing. We then categorise porous carbons based on their pore sizes and the presence or absence of heteroatom doping. Finally, we provide an overview of recent applications of porous carbon materials as electrodes for supercapacitors. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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66 pages, 6730 KiB

Open AccessReview

Gold Nanomaterials-Based Electrochemical Sensors and Biosensors for Phenolic Antioxidants Detection: Recent Advances

by Rita Petrucci, Martina Bortolami, Paola Di Matteo and Antonella Curulli

Nanomaterials 2022, 12(6), 959; https://doi.org/10.3390/nano12060959 - 14 Mar 2022

Cited by 33 | Viewed by 5113

Abstract

Antioxidants play a central role in the development and production of food, cosmetics, and pharmaceuticals, to reduce oxidative processes in the human body. Among them, phenolic antioxidants are considered even more efficient than other antioxidants. They are divided into natural and synthetic. The natural antioxidants are generally found in plants and their synthetic counterparts are generally added as preventing agents of lipid oxidation during the processing and storage of fats, oils, and lipid-containing foods: All of them can exhibit different effects on human health, which are not always beneficial. Because of their relevant bioactivity and importance in several sectors, such as agro-food, pharmaceutical, and cosmetic, it is crucial to have fast and reliable analysis Rmethods available. In this review, different examples of gold nanomaterial-based electrochemical (bio)sensors used for the rapid and selective detection of phenolic compounds are analyzed and discussed, evidencing the important role of gold nanomaterials, and including systems with or without specific recognition elements, such as biomolecules, enzymes, etc. Moreover, a selection of gold nanomaterials involved in the designing of this kind of (bio)sensor is reported and critically analyzed. Finally, advantages, limitations, and potentialities for practical applications of gold nanomaterial-based electrochemical (bio)sensors for detecting phenolic antioxidants are discussed. Full article

(This article belongs to the Special Issue Nanomaterials for Electrochemical Applications)

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