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Synthesis and Characterization of Nanoparticles

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A special issue of Applied Sciences (ISSN 2076-3417). This special issue belongs to the section "Nanotechnology and Applied Nanosciences".

Deadline for manuscript submissions: closed (30 November 2020) | Viewed by 32964

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Special Issue Editors

Dr. Pietro Calandra

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Guest Editor

DSCTM, National Council of Research, Piazzale Aldo Moro, 7, 00185 Rome, Italy
Interests: self-intermolecular interactions; chemistry; physics; materials; literature; science popularization
Special Issues, Collections and Topics in MDPI journals

Dr. Domenico Lombardo

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Guest Editor

Consiglio Nazionale delle Ricerche, Istituto Processi Chimico-Fisici, (CNR–IPCF), 98158 Messina, Italy
Interests: structure and interactuion in nano-colloids (polymers and block copolymers; dendrimers; lipids; proteins); self-assembly in nanostructured (and hybrid) materials; interaction of nanoparticles with model bio-membranes and biomaterials
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Nanoparticles have recently gained increased attention due to their scientific and technological importance: From a scientific point of view, the composition and the atomic order of the aggregates, in addition to size, are pivotal factors in determining their properties, while their novel properties, unknown to bulk materials, are of interest in a huge number of applications, from catalysis to electronics and from optical to magnetic devices.

The main focus of this Special Issue will be to point out the progresses on the nanoscale particles from both a theoretical and experimental point of view: Research articles, with special emphasis to results obtained in the last five years, are welcome, as well as review articles on emerging fields. Potential topics include but are not limited to:

Optical characterizations
Magnetic behavior
Computational structure optimization
Pseudopotentials for quantum mechanical calculations on composite nanoparticles
Catalysis
Plasmonics
Novel applications in chemistry
Models for ordering and self-segregation
Janus particles
Modeling and simulation of structure–properties
Deposition
Surface functionalization
Properties of interfaces between different materials
Drug and gene delivery
Nanocomposites for biomedical applications
Self-assembly and supramolecular ordering
Methods for synthesis of composite nanoparticles
Methods for characterization of composite nanoparticles
Soft nanoparticles
Dendrimers

Dr. Pietro Calandra
Dr. Domenico Lombardo
Guest Editors

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Keywords

nanoparticles
modeling
nanotechnology
nanoscale
synthesis
nanostrctures

Published Papers (10 papers)

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Research

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12 pages, 2382 KiB

Open AccessFeature PaperArticle

Spinel Iron Oxide by the Co-Precipitation Method: Effect of the Reaction Atmosphere

by Sawssen Slimani, Carlo Meneghini, Maryam Abdolrahimi, Alessandro Talone, Jean Pierre Miranda Murillo, Gianni Barucca, Nader Yaacoub, Patrizia Imperatori, Erzsébet Illés, Mourad Smari, Essebti Dhahri and Davide Peddis

Appl. Sci. 2021, 11(12), 5433; https://doi.org/10.3390/app11125433 - 11 Jun 2021

Cited by 19 | Viewed by 2733

Abstract

Synthesis atmosphere (i.e., air and nitrogen) effects on the physical properties and formation mechanism of spinel iron oxide nanoparticles prepared via the co-precipitation method have been investigated using a multi-technique approach. The obtained magnetic nanoparticles (MNPs) were characterized using the X-ray diffraction, transmission electron microscopy (TEM), SQUID magnetometry, Mössbauer spectroscopy and X-ray absorption near-edge Structure spectroscopy techniques. The synthesis procedure leads to the formation of a spinel structure with an average crystallite size of 9.0(9) nm. The morphology of the particles synthetized under an inert atmosphere was quasi-spherical, while the nanoparticles prepared in air present a faceted shape. The small differences observed in morphological properties are explained by the influence of the reaction atmosphere on the formation mechanism of the MNPs. The magnetic characterization indicates that both samples exhibit superparamagnetic behavior at 300 K. The investigation by means of the Langevin approach at 300 K also leads to equal values for the mean size of the magnetic cores (D_m). Additionally, the analysis of the Mössbauer spectra revealed the lack of spin disorder for both samples, resulting in a high saturation magnetization. The fit of XANES spectrum suggests that about 2/3 of the iron ions reside in a local environment close to that of γ-Fe₂O₃ and about 1/3 close to that of Fe₃O₄ for the sample synthetized in inert atmosphere. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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16 pages, 1347 KiB

Open AccessFeature PaperArticle

Preparation of Asphalt Concretes by Gyratory Compactor: A Case of Study with Rheological and Mechanical Aspects

by Paolino Caputo, Pietro Calandra, Rosolino Vaiana, Vincenzo Gallelli, Giovanni De Filpo and Cesare Oliviero Rossi

Appl. Sci. 2020, 10(23), 8567; https://doi.org/10.3390/app10238567 - 30 Nov 2020

Cited by 6 | Viewed by 2030

Abstract

For asphalt concrete preparation in laboratory mix-design operations, bitumens are usually mixed with micrometer-sized particles (filler), sand and centimeter-sized crushed stones in a gyratory press at a temperature of about 140–155 °C depending on the bitumen viscosity, until adequate homogenization and compaction take place (air voids optimum). This requires energy consumption. To minimize it, the process needs to be optimized and is usually made empirically. The aim of this manuscript is to gain a comprehension of the physico-chemical mechanisms involved in the process by exploring: (i) the rheological properties (viscosity, activation energy) of a neat and RTFOT-aged bitumen, in presence and in absence of a filler, (ii) the volumetric and resistance behavior under the compaction in a standard Gyratory Compactor (GC) of their blends with aggregates and (iii) the mechanical properties (Indirect Tensile Strength, compression and tensile deformation) of the final products. Correlations between activation energy and pre-exponential factor of the viscosity on a side, and between viscosity, workability and final mechanical properties on the other side allowed to provide a rational interpretation of the physico-chemical processes involved in the framework of the physics of complex fluids. The scientific clues will be of help in optimizing the workability in asphalt concretes productions with obvious repercussions in terms of energy savings, useful for economic and environmental issues. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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18 pages, 23220 KiB

Open AccessFeature PaperArticle

Preparation and Characterization of Gold Nanorods Coated with Gellan Gum and Lipoic Acid

by Paola Varvarà, Luigi Tranchina, Gennara Cavallaro and Mariano Licciardi

Appl. Sci. 2020, 10(23), 8322; https://doi.org/10.3390/app10238322 - 24 Nov 2020

Cited by 7 | Viewed by 1958

Abstract

Gold nanorods (AuNRs) can combine therapeutic hyperthermia with diagnostic features, representing a smart choice to address personalized cancer treatments. In this regard, a crucial quest is the selection of the right biocompatible coating agent able to stabilize them in the physiological environment, further endowing the possibility to load bioactive molecules and/or targeting moieties. Therefore, AuNRs optical properties can be successfully merged with advantageous materials features to obtain selective photothermal therapy (PTT) systems. Here, the natural materials lipoic acid (LA) and the polysaccharide gellan gum (GG) were chosen to prepare three types of stabilized gold nanorods, using LA (AuNRs/LA), a layered coating of LA and GG (AuNRs/LA,GG) or a newly synthesized covalent derivative of LA and GG (AuNRs/GG-LA). The samples displayed diverse stability and dispersibility. Hydrodynamic diameters and surface potential analyses confirmed the nanometric size (100–200 nm) and showed surface charges ranging from +19.5 to −25.6 mV. Particular attention was thus paid to analyze the differences between hyperthermia properties exhibited after near-infrared (NIR) laser irradiation. Furthermore, the cytocompatibility and photothermal effect were tested on HCT116 human colon cancer cell line. Collected data have finally allowed selecting AuNRs/LA,GG as the best candidate for possible use in PTT of cancer. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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15 pages, 4288 KiB

Open AccessFeature PaperArticle

Sulfonated Cellulose-Based Magnetic Composite as Useful Media for Water Remediation from Amine Pollutants

by Antonio De Nino, Matteo Antonio Tallarida, Vincenzo Algieri, Fabrizio Olivito, Paola Costanzo, Giovanni De Filpo and Loredana Maiuolo

Appl. Sci. 2020, 10(22), 8155; https://doi.org/10.3390/app10228155 - 18 Nov 2020

Cited by 17 | Viewed by 2913

Abstract

Commercially available microcrystalline cellulose (MCC) was functionalized using chlorosulfonic acid, while iron oxide nanoparticles (IONPs) were adsorbed on the surface of the cellulose derivative by the Massart’s co-precipitation method. The obtained magnetite-decorated sulfate cellulose nanoparticles (MDSCNs) were characterized via Fourier transform infrared (FTIR) spectroscopy, scanning-electron microscopy (SEM), and elemental analysis, while the acidity of the functionalized cellulose was determined using an acid–base titration with phenolphthalein as an indicator. Furthermore, in order to determine the adsorptive power of the obtained composite, a series of analyses were performed on aqueous amine pollutants using flame ionization detection gas chromatography (GC-FID). The results of this study clearly show how a bio-compatible green polymer as cellulose can be easy functionalized in order to improve its chemical and physical properties, obtaining a magnetic composite useful in water purification. Adsorption percentages up to 90% and a very small amount of composite used (100 mg) proved how our material can be a powerful tool in environmental remediation. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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11 pages, 5017 KiB

Open AccessFeature PaperArticle

Functionalization and Modification of Bitumen by Silica Nanoparticles

by Ainur Zhambolova, Anna Lisa Vocaturo, Yerbol Tileuberdi, Yerdos Ongarbayev, Paolino Caputo, Iolinda Aiello, Cesare Oliviero Rossi and Nicolas Godbert

Appl. Sci. 2020, 10(17), 6065; https://doi.org/10.3390/app10176065 - 01 Sep 2020

Cited by 9 | Viewed by 2231

Abstract

A study on the effect of silica nanoparticles (SNPs) dispersion in bitumen is herein reported. First, the size of the nanoparticles was finely tuned by controlling the experimental conditions during their synthesis, obtaining spherical SNPs with diameter ranging from 95 up to 900 nm. Subsequently, SNPs were embedded with peripheral amine groups by using APTES (3-aminopropyltriethoxysilane) as functionalized agent (NH₂@SNP), and ultimately long alkyl chains were grafted by reacting the free amine with an alkylated aldehyde (C₁₄N@SNP). All SNPs (ca. 1 wt%.) were dispersed in bitumen to probe their effect on the rheological properties of bitumen. No significant change in the thermorheological properties of bitumen was observed upon varying the size of the SNPs. Slight improvement was observed when using NH₂@SNPs, while the best results were obtained by using C₁₄N@SNPs, showing the crucial role that hydrophobic substituents play in bitumen binders which leads to significant improvements. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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18 pages, 3369 KiB

Open AccessArticle

Silica-Coated Magnetic Nanocomposites for Pb²⁺ Removal from Aqueous Solution

by Roxana Nicola, Otilia Costişor, Mihaela Ciopec, Adina Negrea, Radu Lazău, Cătălin Ianăşi, Elena-Mirela Picioruş, Adél Len, László Almásy, Elisabeta I. Szerb and Ana-Maria Putz

Appl. Sci. 2020, 10(8), 2726; https://doi.org/10.3390/app10082726 - 15 Apr 2020

Cited by 46 | Viewed by 3095

Abstract

Magnetic iron oxide-silica shell nanocomposites with different iron oxide/silica ratio were synthesized and structurally characterized by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), small-angle neutron scattering, magnetic and N₂-sorption studies. The composite that resulted with the best properties in terms of contact surface area and saturation of magnetization was selected for Pb²⁺ adsorption studies from aqueous media. The material presented good absorption capacity (maximum adsorption capacity 14.9 mg·g⁻¹) comparable with similar materials presented in literature. Its chemico-physical stability and adsorption capacity recommend the nanocomposite as a cheap adsorbent material for lead. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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13 pages, 2567 KiB

Open AccessArticle

Effect of Calcination Temperature on Photocatalytic Activity of Synthesized TiO₂ Nanoparticles via Wet Ball Milling Sol-Gel Method

by Siripond Phromma, Tuksadon Wutikhun, Panita Kasamechonchung, Tippabust Eksangsri and Chaweewan Sapcharoenkun

Appl. Sci. 2020, 10(3), 993; https://doi.org/10.3390/app10030993 - 03 Feb 2020

Cited by 80 | Viewed by 7698

Abstract

In this work, TiO₂ nanoparticles were successfully synthesized with narrow size distribution via a wet ball milling sol-gel method. The effect of calcination temperature on photocatalytic activity was observed from particle size, crystallite size, and phase transition of TiO₂ nanoparticles. Increasing calcination temperature increased particle size, crystallite size, and the crystallinity of synthesized TiO₂. Phase transition depended on variation in calcination temperatures. A two-phase mixture of anatase and brookite was obtained with lower calcination temperature whereas a three-phase mixture appeared when calcination temperature was 500–600 °C. With higher temperature, the rutile phase kept increasing until it was the only phase observed at 800 °C. Anatase strongly affected the photocatalytic activity from 300 °C to 600 °C while the particle size of TiO₂ was found to have a dominant effect on the photocatalytic activity between 600 °C and 700 °C. A mixture of three phases of TiO₂-600 exhibited the highest methylene blue degradation with the rate constant of 9.46 × 10⁻² h⁻¹ under ultraviolet (UV) irradiation. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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14 pages, 2536 KiB

Open AccessArticle

Optical Birefringence Growth Driven by Magnetic Field in Liquids: The Case of Dibutyl Phosphate/Propylamine System

by Mikolaj Pochylski, Domenico Lombardo and Pietro Calandra

Appl. Sci. 2020, 10(1), 164; https://doi.org/10.3390/app10010164 - 24 Dec 2019

Cited by 12 | Viewed by 2244

Abstract

Magnetically-induced birefringence is usually low in molecular liquids owing to the low magnetic energy of molecules with respect to the thermal one. Despite this, it has been found that a mixture of dibutyl phosphate and propylamine at propylamine molar ratio (X) around 0.33 surprisingly gives an intense effect (∆n/λ ≈ −0.1 at 1 Tesla). In this paper the time- and intensity- response to the magnetic field of such mixture have been studied. It was found that the reaction to the magnetic field is unusually slow (from several minutes to hours) depending of the magnetic field intensity. On the basis of the data, the model of orientable dipoles dispersed in a matrix enables to interpret the magnetic field-induced self-assembly in terms of soft molecules-based nanostructures. The analogy with systems made of magnetically polarizable (solid or soft) particles dispersed in liquid carrier allows understanding, at the microscopic scale, the molecular origin and the supra-molecular dynamics involved in the observed behavior. The data present a novel phenomenon in liquid phase where the progressive building up/change of ordered and strongly interacting amphiphiles is driven by the magnetic field. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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10 pages, 583 KiB

Open AccessArticle

Soft Cationic Nanoparticles for Drug Delivery: Production and Cytotoxicity of Solid Lipid Nanoparticles (SLNs)

by Amélia M. Silva, Carlos Martins-Gomes, Tiago E. Coutinho, Joana F. Fangueiro, Elena Sanchez-Lopez, Tatiana N. Pashirova, Tatiana Andreani and Eliana B. Souto

Appl. Sci. 2019, 9(20), 4438; https://doi.org/10.3390/app9204438 - 19 Oct 2019

Cited by 44 | Viewed by 4548

Abstract

The surface properties of nanoparticles have decisive influence on their interaction with biological barriers (i.e., living cells), being the concentration and type of surfactant factors to have into account. As a result of different molecular structure, charge, and degree of lipophilicity, different surfactants may interact differently with the cell membrane exhibiting different degrees of cytotoxicity. In this work, the cytotoxicity of two cationic solid lipid nanoparticles (SLNs), differing in the cationic lipids used as surfactants CTAB (cetyltrimethylammonium bromide) or DDAB (dimethyldioctadecylammonium bromide), referred as CTAB-SLNs and DDAB-SLNs, respectively, was assessed against five different human cell lines (Caco-2, HepG2, MCF-7, SV-80, and Y-79). Results showed that the cationic lipids used in SLN production highly influenced the cytotoxic profile of the particles, with CTAB-SLNs being highly cytotoxic even at low concentrations (IC₅₀ < 10 µg/mL, expressed as CTAB amount). DDAB-SLNs produced much lower cytotoxicity, even at longer exposure time (IC₅₀ from 284.06 ± 17.01 µg/mL (SV-80) to 869.88 ± 62.45 µg/mL (MCF-7), at 48 h). To the best of our knowledge, this is the first report that compares the cytotoxic profile of CTAB-SLNs and DDAB-SLNs based on the concentration and time of exposure, using different cell lines. In conclusion, the choice of the right surfactant for biological applications influences the biocompatibility of the nanoparticles. Regardless the type of drug delivery system, not only the cytotoxicity of the drug-loaded nanoparticles should be assessed, but also the blank (non-loaded) nanoparticles as their surface properties play a decisive role both in vitro and in vivo. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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28 pages, 3539 KiB

Open AccessCommentary

Exploiting Nanoparticles to Improve the Properties of Bitumens and Asphalts: At What Extent Is It Really Worth It?

by Pietro Calandra, Valeria Loise, Michele Porto, Cesare Oliviero Rossi, Domenico Lombardo and Paolino Caputo

Appl. Sci. 2020, 10(15), 5230; https://doi.org/10.3390/app10155230 - 29 Jul 2020

Cited by 11 | Viewed by 2533

Abstract

Asphalt concretes are materials used worldwide. It is well-known that in such materials the minor component, the bitumen, plays the most important role since it binds the high fraction (>95%) of inorganic macrometer-sized particles ensuring a coherent material fit for uses in road pavement. Additives can be used to increase the overall rheological properties, with high benefits in terms of resistance to mechanical stress and to ageing. Among these, nanoparticles have recently been considered as very effective additives in increasing the overall performance, increasing the viscosity, the rutting parameter and the recovery from deformation. However, they are expensive, so a delicate equilibrium between costs and benefits must be found for large-scale uses. In this framework, we furnish our critical analysis of the state-of-the art technologies used for improving the bitumen performances by means of nanoparticles with an eye to eventual added-values (like anti-oxidant effect, antistripping properties, or UV radiation screening which avoids radiation-induced ageing…). We will critically consider the costs involved in their use and we will give our opinion about vanguard techniques which can be fit for the analysis of nanoparticles-containing bitumens and asphalts. Interesting perspectives will be also given for future research and applications. Full article

(This article belongs to the Special Issue Synthesis and Characterization of Nanoparticles)

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