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Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis
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Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis

A special issue of Materials (ISSN 1996-1944).

Deadline for manuscript submissions: closed (31 July 2016) | Viewed by 57558

Special Issue Editors

Prof. Dr. Andrea P. Reverberi

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Guest Editor
DCCI—Department of Chemistry and Industrial Chemistry, Faculty of Sciences, University of Genova, Via Dodecaneso 31, 16146 Genova, Italy
Interests: nanotechnology and nanoparticles chemical synthesis (bottom-up processes, top-down processes); solids disaggregation and etching (chemical etching, templated etching, and mask etching); lithography (stencil lithography, nanolithography); nano-manufacturing (patterning, nanomachining); modelling of heat and mass transfer in condensed matter
Special Issues, Collections and Topics in MDPI journals
Dr. Marco Salerno

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Guest Editor
Department of Functional Materials and Hydrogen Technology, Military University of Technology, Warsaw, Poland
Interests: scanning probe microscopy; nanocomposites; nanoporous oxides of valve metals; applications of anodic porous alumina; SERS; biocompatibility of materials; nanoindentation; dental restorative materials and implants
Special Issues, Collections and Topics in MDPI journals

Special Issue Information

Dear Colleagues,

Inorganic nanoparticles have assumed a key role in many interdisciplinary fields, such as physics, engineering, and medicine. The present Special Issue addresses a broad variety of techniques, aiming at synthesizing inorganic nanoparticles by chemical reactions in liquid phase and physical processes, including precipitation, thermal dissociation, redox reactions, laser ablation, surface disaggregation, and other methods where chemistry and physics of nanoparticles production are strictly interconnected.

This choice is motivated by the need of finding new manufacturing protocols, matching both yield and reliability of the synthesis process with an improved quality of the final product in terms of shape, dimensions and stability of the nanosized phase.

We warmly invite all researchers interested in such a topic to present full papers, communications and reviews.

Andrea P. Reverberi
Marco Salerno
Guest Editors

Manuscript Submission Information

Manuscripts should be submitted online at www.mdpi.com by registering and logging in to this website. Once you are registered, click here to go to the submission form. Manuscripts can be submitted until the deadline. All submissions that pass pre-check are peer-reviewed. Accepted papers will be published continuously in the journal (as soon as accepted) and will be listed together on the special issue website. Research articles, review articles as well as short communications are invited. For planned papers, a title and short abstract (about 100 words) can be sent to the Editorial Office for announcement on this website.

Submitted manuscripts should not have been published previously, nor be under consideration for publication elsewhere (except conference proceedings papers). All manuscripts are thoroughly refereed through a single-blind peer-review process. A guide for authors and other relevant information for submission of manuscripts is available on the Instructions for Authors page. Materials is an international peer-reviewed open access semimonthly journal published by MDPI.

Please visit the Instructions for Authors page before submitting a manuscript. The Article Processing Charge (APC) for publication in this open access journal is 2600 CHF (Swiss Francs). Submitted papers should be well formatted and use good English. Authors may use MDPI's English editing service prior to publication or during author revisions.

Keywords

  • inorganic nanoparticles
  • wet-chemical methods
  • physical methods
  • reaction kinetics
  • capping agents and surfactants
  • bottom-up methods
  • top-down methods
  • nanoparticles separation

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Published Papers (7 papers)

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Research

2268 KiB  
Article
Synthesis of Fluorescent Core-Shell Metal Nanohybrids: A Versatile Approach
by Marina Alloisio, Melania Rusu, Stefano Ottonello, Massimo Ottonelli, Sergio Thea and Davide Comoretto
Materials 2016, 9(12), 997; https://doi.org/10.3390/ma9120997 - 9 Dec 2016
Cited by 5 | Viewed by 4842
Abstract
A flexible way of fabricating core-shell noble metal-organic nanohybrids with tailored chemical and spectroscopic properties is proposed here. The synthetic protocol consists of a multi-step procedure able to guarantee acceptable reproducibility of core size and shape as well as control of the organic [...] Read more.
A flexible way of fabricating core-shell noble metal-organic nanohybrids with tailored chemical and spectroscopic properties is proposed here. The synthetic protocol consists of a multi-step procedure able to guarantee acceptable reproducibility of core size and shape as well as control of the organic outer layer. The proposed method highlights limitations in obtaining highly controllable products, although the heterogeneity degree of the nanostructures is in line with that expected from bottom-up approaches in solution. Selective functionalization of the nanohybrids with properly-substituted fluorescent dyes under variable experimental conditions allowed the preparation of composite systems of tunable spectroscopic properties to be employed as nanoprobes in sensing or photonic applications. To this end, preliminary investigation on embedding the nanohybrids in compatible polymeric matrices is also reported. Full article
(This article belongs to the Special Issue Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis)
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5837 KiB  
Article
Functionalization of Fe3O4 NPs by Silanization: Use of Amine (APTES) and Thiol (MPTMS) Silanes and Their Physical Characterization
by Silvia Villa, Paola Riani, Federico Locardi and Fabio Canepa
Materials 2016, 9(10), 826; https://doi.org/10.3390/ma9100826 - 12 Oct 2016
Cited by 105 | Viewed by 14808
Abstract
In this paper the results concerning the synthesis of magnetite (Fe3O4) nanoparticles (NPs), their functionalization using silane derivatives, such as (3-Aminopropyl)triethoxysilane (APTES) and (3-mercaptopropyl)trimethoxysilane (MPTMS), and their exhaustive morphological and physical characterization by field emission scanning electron microscopy (FE-SEM) [...] Read more.
In this paper the results concerning the synthesis of magnetite (Fe3O4) nanoparticles (NPs), their functionalization using silane derivatives, such as (3-Aminopropyl)triethoxysilane (APTES) and (3-mercaptopropyl)trimethoxysilane (MPTMS), and their exhaustive morphological and physical characterization by field emission scanning electron microscopy (FE-SEM) with energy dispersion X-ray spectrometer (EDX) analysis, AC magnetic susceptibility, UV-VIS and IR spectroscopy, and thermogravimetric (TGA) analyses are reported. Two different paths were adopted to achieve the desired functionalization: (1) the direct reaction between the functionalized organo-silane molecule and the surface of the magnetite nanoparticle; and (2) the use of an intermediate silica coating. Finally, the occurrence of both the functionalization with amino and thiol groups has been demonstrated by the reaction with ninhydrin and the capture of Au NPs, respectively. Full article
(This article belongs to the Special Issue Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis)
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4483 KiB  
Article
Mesquite Gum as a Novel Reducing and Stabilizing Agent for Modified Tollens Synthesis of Highly Concentrated Ag Nanoparticles
by Maira Berenice Moreno‐Trejo and Margarita Sánchez‐Domínguez
Materials 2016, 9(10), 817; https://doi.org/10.3390/ma9100817 - 4 Oct 2016
Cited by 21 | Viewed by 6348
Abstract
The synthesis that is described in this study is for the preparation of silver nanoparticles of sizes ranging from 10 nm to 30 nm with a defined shape (globular), confirmed by UV-vis, SEM, STEM and DLS analysis. This simple and favorable one-step modified [...] Read more.
The synthesis that is described in this study is for the preparation of silver nanoparticles of sizes ranging from 10 nm to 30 nm with a defined shape (globular), confirmed by UV-vis, SEM, STEM and DLS analysis. This simple and favorable one-step modified Tollens reaction does not require any special equipment or other stabilizing or reducing agent except for a solution of purified mesquite gum, and it produces aqueous colloidal dispersions of silver nanoparticles with a stability thatexceeds three months, a relatively narrow size distribution, a low tendency to aggregate and a yield of at least 95% for all cases. Reaction times are between 15 min and 60 min to obtain silver nanoparticles in concentrations ranging from 0.1 g to 3 g of Ag per 100 g of reaction mixture. The proposed synthetic method presents a high potential for scale-up, since its production capacity is rather high and the methodology is simple.The synthesis that is described in this study is for the preparation of silver nanoparticles of sizes ranging from 10 nm to 30 nm with a defined shape (globular), confirmed by UV-vis, SEM, STEM and DLS analysis. This simple and favorable one-step modified Tollens reaction does not require any special equipment or other stabilizing or reducing agent except for a solution of purified mesquite gum, and it produces aqueous colloidal dispersions of silver nanoparticles with a stability thatexceeds three months, a relatively narrow size distribution, a low tendency to aggregate and a yield of at least 95% for all cases. Reaction times are between 15 min and 60 min to obtain silver nanoparticles in concentrations ranging from 0.1 g to 3 g of Ag per 100 g of reaction mixture. The proposed synthetic method presents a high potential for scale-up, since its production capacity is rather high and the methodology is simple. Full article
(This article belongs to the Special Issue Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis)
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2572 KiB  
Article
Synthesis of Copper Nanoparticles in Ethylene Glycol by Chemical Reduction with Vanadium (+2) Salts
by Andrea Pietro Reverberi, Marco Salerno, Simone Lauciello and Bruno Fabiano
Materials 2016, 9(10), 809; https://doi.org/10.3390/ma9100809 - 29 Sep 2016
Cited by 50 | Viewed by 9597
Abstract
Copper nanoparticles have been synthesized in ethylene glycol (EG) using copper sulphate as a precursor and vanadium sulfate as an atypical reductant being active at room temperature. We have described a technique for a relatively simple preparation of such a reagent, which has [...] Read more.
Copper nanoparticles have been synthesized in ethylene glycol (EG) using copper sulphate as a precursor and vanadium sulfate as an atypical reductant being active at room temperature. We have described a technique for a relatively simple preparation of such a reagent, which has been electrolytically produced without using standard procedures requiring an inert atmosphere and a mercury cathode. Several stabilizing agents have been tested and cationic capping agents have been discarded owing to the formation of complex compounds with copper ions leading to insoluble phases contaminating the metallic nanoparticles. The elemental copper nanoparticles, stabilized with polyvinylpyrrolidone (PVP) and sodium dodecyl sulphate (SDS), have been characterized for composition by energy dispersive X-ray spectroscopy (EDS), and for size by dynamic light scattering (DLS), and transmission electron microscopy (TEM), giving a size distribution in the range of 40–50 nm for both stabilizing agents. From a methodological point of view, the process described here may represent an alternative to other wet-chemical techniques for metal nanoparticle synthesis in non-aqueous media based on conventional organic or inorganic reductants. Full article
(This article belongs to the Special Issue Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis)
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1676 KiB  
Article
Extensive Characterization of Oxide-Coated Colloidal Gold Nanoparticles Synthesized by Laser Ablation in Liquid
by Romuald Intartaglia, Marina Rodio, Mohamed Abdellatif, Mirko Prato and Marco Salerno
Materials 2016, 9(9), 775; https://doi.org/10.3390/ma9090775 - 14 Sep 2016
Cited by 17 | Viewed by 5869
Abstract
Colloidal gold nanoparticles are a widespread nanomaterial with many potential applications, but their aggregation in suspension is a critical issue which is usually prevented by organic surfactants. This solution has some drawbacks, such as material contamination and modifications of its functional properties. The [...] Read more.
Colloidal gold nanoparticles are a widespread nanomaterial with many potential applications, but their aggregation in suspension is a critical issue which is usually prevented by organic surfactants. This solution has some drawbacks, such as material contamination and modifications of its functional properties. The gold nanoparticles presented in this work have been synthesized by ultra-fast laser ablation in liquid, which addresses the above issues by overcoating the metal nanoparticles with an oxide layer. The main focus of the work is in the characterization of the oxidized gold nanoparticles, which were made first in solution by means of dynamic light scattering and optical spectroscopy, and then in dried form by transmission electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy, and finally by surface potential measurements with atomic force microscopy. The light scattering assessed the nanoscale size of the formed particles and provided insight in their stability. The nanoparticles’ size was confirmed by direct imaging in transmission electron microscopy, and their crystalline nature was disclosed by X-ray diffraction. The X-ray photoelectron spectroscopy showed measurements compatible with the presence of surface oxide, which was confirmed by the surface potential measurements, which are the novel point of the present work. In conclusion, the method of laser ablation in liquid for the synthesis of gold nanoparticles has been presented, and the advantage of this physical approach, consisting of coating the nanoparticles in situ with gold oxide which provides the required morphological and chemical stability without organic surfactants, has been confirmed by using scanning Kelvin probe microscopy for the first time. Full article
(This article belongs to the Special Issue Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis)
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1463 KiB  
Article
Enhancement of TiO2 NPs Activity by Fe3O4 Nano-Seeds for Removal of Organic Pollutants in Water
by Silvia Villa, Valentina Caratto, Federico Locardi, Stefano Alberti, Michela Sturini, Andrea Speltini, Federica Maraschi, Fabio Canepa and Maurizio Ferretti
Materials 2016, 9(9), 771; https://doi.org/10.3390/ma9090771 - 10 Sep 2016
Cited by 21 | Viewed by 6282
Abstract
The enhancement of the photocatalytic activity of TiO2 nanoparticles (NPs), synthesized in the presence of a very small amount of magnetite (Fe3O4) nanoparticles, is here presented and discussed. From X-ray diffraction (XRD) and differential scanning calorimetry (DSC) analyses, [...] Read more.
The enhancement of the photocatalytic activity of TiO2 nanoparticles (NPs), synthesized in the presence of a very small amount of magnetite (Fe3O4) nanoparticles, is here presented and discussed. From X-ray diffraction (XRD) and differential scanning calorimetry (DSC) analyses, the crystallinity of TiO2 nanoparticles (NPs) seems to be affected by Fe3O4, acting as nano-seeds to improve the tetragonal TiO2 anatase structure with respect to the amorphous one. Photocatalytic activity data, i.e., the degradation of methylene blue and the Ofloxacin fluoroquinolone emerging pollutant, give evidence that the increased crystalline structure of the NPs, even if correlated to a reduced surface to mass ratio (with respect to commercial TiO2 NPs), enhances the performance of this type of catalyst. The achievement of a relatively well-defined crystal structure at low temperatures (Tmax = 150 °C), preventing the sintering of the TiO2 NPs and, thus, preserving the high density of active sites, seems to be the keystone to understand the obtained results. Full article
(This article belongs to the Special Issue Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis)
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20347 KiB  
Article
Synthesis of Mixed Cu/Ce Oxide Nanoparticles by the Oil-in-Water Microemulsion Reaction Method
by Kelly Pemartin-Biernath, Andrea V. Vela-González, Maira B. Moreno-Trejo, César Leyva-Porras, Iván E. Castañeda-Reyna, Isaías Juárez-Ramírez, Conxita Solans and Margarita Sánchez-Domínguez
Materials 2016, 9(6), 480; https://doi.org/10.3390/ma9060480 - 16 Jun 2016
Cited by 23 | Viewed by 8556
Abstract
Cerium oxide and mixed Cu/Ce oxide nanoparticles were prepared by the oil-in-water (O/W) microemulsion reaction method in mild conditions. The Cu/Ce molar ratio was varied between 0/100 and 50/50. According to X-ray diffraction (XRD), below 30/70 Cu/Ce molar ratio, the materials presented a [...] Read more.
Cerium oxide and mixed Cu/Ce oxide nanoparticles were prepared by the oil-in-water (O/W) microemulsion reaction method in mild conditions. The Cu/Ce molar ratio was varied between 0/100 and 50/50. According to X-ray diffraction (XRD), below 30/70 Cu/Ce molar ratio, the materials presented a single phase consistent with cubic fluorite CeO2. However, above Cu/Ce molar ratio 30/70, an excess monoclinic CuO phase in coexistence with the predominant Cu/Ce mixed oxide was detected by XRD and High-Resolution Transmission Electron Microscopy (HRTEM). Raman spectroscopy showed that oxygen vacancies increased significantly as the Cu content was increased. Band gap (Eg) was investigated as a function of the Cu/Ce molar ratio, resulting in values from 2.91 eV for CeO2 to 2.32 eV for the mixed oxide with 30/70 Cu/Ce molar ratio. These results indicate that below 30/70 Cu/Ce molar ratio, Cu2+ is at least partially incorporated into the ceria lattice and very well dispersed in general. In addition, the photodegradation of Indigo Carmine dye under visible light irradiation was explored for selected samples; it was shown that these materials can remove such contaminants, either by adsorption and/or photodegradation. The results obtained will encourage investigation into the optical and photocatalytic properties of these mixed oxides, for widening their potential applications. Full article
(This article belongs to the Special Issue Advances in Physical and Wet-Chemical Methods for Inorganic Nanoparticles Synthesis)
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