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Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles

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A special issue of Nanomaterials (ISSN 2079-4991). This special issue belongs to the section "Synthesis, Interfaces and Nanostructures".

Deadline for manuscript submissions: closed (31 December 2019) | Viewed by 38741

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Prof. Dr. Ammar Souad

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ITODYS Laboratory, Chemistry Department, Universite Paris Diderot, 75205 Paris, France
Interests: Elaboration of chemically, structurally, and microstructurally controlled inorganic homo- and hetero-architected nanoparticles (metals, hydroxides, alkoxides, oxides, chalcogenides, halogenides, etc.) using the polyol process; Elucidation of the involved nanoparticle nucleation and growth mechanisms in solution, correlating the polyol synthesis conditions to the physico-biochemical nanoparticle properties; Nanoparticle design for electromagnetic-based technological applications in the field of renewable energy, biomedicine, or telecommunication.

Prof. Dr. Fernand Fievet

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Guest Editor

ITODYS Laboratory, Chemistry Department, Universite Paris Diderot, 75205 Paris, France
Interests: Elaboration of chemically, structurally, and microstructurally controlled inorganic nanoparticles (metals, hydroxides, alkoxides, oxides, chalcogenides, halogenides, etc.) using the polyol process; Elucidation of the involved nanoparticle nucleation and growth mechanisms in solution, correlating the polyol synthesis conditions to the physico-biochemical nanoparticle properties

Special Issue Information

Dear Colleagues,

Polyol synthesis has emerged these last years as a powerful and scalable wet-chemistry route for the production of chemically and structurally controlled inorganic nanoparticles. Through a simple optimization of the operating synthesis conditions, it allows the design of well-shaped homo- and hetero-nanostructured metal, oxide, chalcogenide, halogenide, alkoxide, or hydroxide particles, with a great applicative interest for various technological fields, including renewable energy, human health, environment, telecommunications.

This Special Issue invites manuscripts concerning the synthesis of such functional nanoparticles, their characterization and upscaling with a particular emphasis on their applications through their integration in targeted electromagnetic-based devices. Original articles on synthesis strategies will be considered, including the preparation of metastable phases, original microtructures (nanoflowers, core-shell, hetero-coagulate, janus system, etc.), new compounds (carbon dots, etc.), and in situ nanohybrids (self-assembly in polyol, etc.). Articles describing polyol-made nanoparticle shaping (nanoconsolidates, functional inks, thin films, ferrofluids, etc.) and their succesful use in different technological and biotechnological fields are also recommended.

Prof. Dr. Ammar Souad
Prof. Dr. Fernand Fievet
Guest Editors

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Keywords

Inorganic nanoparticles
Nucleation and growth mechanisms
Synthesis upscaling
Nanohybrides
Nanoparticles self-assembly
Functional nanomaterials

Published Papers (12 papers)

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Editorial

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8 pages, 225 KiB

Open AccessEditorial

Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles

by Souad Ammar and Fernand Fiévet

Nanomaterials 2020, 10(6), 1217; https://doi.org/10.3390/nano10061217 - 22 Jun 2020

Cited by 35 | Viewed by 5633

Abstract

The term “polyol process” was first used in the late eighties by Fiévet, Lagier, and Figlarz [...] Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

Research

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17 pages, 5608 KiB

Open AccessFeature PaperArticle

Polyol-Made Luminescent and Superparamagnetic β-NaY_0.8Eu_0.2F₄@γ-Fe₂O₃ Core-Satellites Nanoparticles for Dual Magnetic Resonance and Optical Imaging

by Walid Mnasri, Lotfi Ben Tahar, Patricia Beaunier, Darine Abi Haidar, Michel Boissière, Olivier Sandre and Souad Ammar

Nanomaterials 2020, 10(2), 393; https://doi.org/10.3390/nano10020393 - 23 Feb 2020

Cited by 7 | Viewed by 3073

Abstract

Red luminescent and superparamagnetic β-NaY_0.8Eu_0.2F₄@γ-Fe₂O₃ nanoparticles, made of a 70 nm-sized β-NaY_0.8Eu_0.2F₄ single crystal core decorated by a 10 nm-thick polycrystalline and discontinuous γ-Fe₂O₃ shell, have been synthesized by the polyol process. Functionalized with citrate ligands they show a good colloidal stability in water making them valuable for dual magnetic resonance and optical imaging or image-guided therapy. They exhibit a relatively high transverse relaxivity r₂ = 42.3 mM⁻¹·s⁻¹ in water at 37 °C, for an applied static magnetic field of 1.41 T, close to the field of 1.5 T applied in clinics, as they exhibit a red emission by two-photon excited fluorescence microscopy. Finally, when brought into contact with healthy human foreskin fibroblast cells (BJH), for doses as high as 50 µg·mL⁻¹ and incubation time as long as 72 h, they do not show evidence of any accurate cytotoxicity, highlighting their biomedical applicative potential. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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14 pages, 5666 KiB

Open AccessArticle

Enhanced Magnetic Behavior of Cobalt Nano-Rods Elaborated by the Polyol Process Assisted with an External Magnetic Field

by Mohamed Ali Bousnina, Amel Dakhlaoui-Omrani, Frédéric Schoenstein, Yaghoub Soumare, Aliou Hamady Barry, Jean-Yves Piquemal, Guillaume Viau, Silvana Mercone and Noureddine Jouini

Nanomaterials 2020, 10(2), 334; https://doi.org/10.3390/nano10020334 - 15 Feb 2020

Cited by 6 | Viewed by 3037

Abstract

Cobalt nano-rods with the hexagonal close-packed (hcp) structure were prepared by reduction of the long-chain carboxylate Co (II) precursor in polyol. The application of an external magnetic field (µ₀H = 1.25 T) during the nucleation and growth steps resulted in a noticeable modification of the mean aspect ratio (length/diameter) of the particles. The particle morphology was also modified as the nano-rods did not exhibit conical heads at their extremities anymore, which are observed for particles prepared without application of an external magnetic field. Besides, the stacking faults density along the c axis of the hcp structure in the cobalt nano-rods has been found to decrease with the increase in the applied magnetic field. The coercive field of randomly oriented nano-rods increased with the aspect ratio, showing the highest value (i.e., 5.8 kOe at 300 K) for the cobalt nano-rods obtained under the highest applied magnetic field. For partially oriented Co nano-rods in toluene solution, the magnetic properties were significantly enhanced with a coercive field of 7.2 kOe at 140 K, while the magnetization saturation reached 92% of the bulk. The M_R/M_S value was about 0.8, indicating a good orientation of the anisotropic particles relative to each other, making them suitable for the preparation of permanent magnets via a bottom-up approach. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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7 pages, 5272 KiB

Open AccessArticle

Synthesis of Magnetic Wires from Polyol-Derived Fe-Glycolate Wires

by Shun Fujieda, Thomas Gaudisson, Jean-Marc Grenèche, Michel François and Souad Ammar

Nanomaterials 2020, 10(2), 318; https://doi.org/10.3390/nano10020318 - 13 Feb 2020

Cited by 1 | Viewed by 2084

Abstract

Fe-glycolate wires with micrometer-scale lengths can be synthesized by the polyol process. Although the as-produced wires are in the paramagnetic state at room temperature, they are transformed into ferrimagnetic iron oxides and ferromagnetic metallic iron wires by reductive annealing. The shape of the wires is unchanged by reductive annealing, and it is possible to control the magnetic properties of the resulting wire-shaped ferri/ferromagnets by adjusting the annealing conditions. Consequently, the reductive annealing of polyol-derived Fe-glycolate wires is an effective material-processing route for the production of magnetic wires. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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13 pages, 2897 KiB

Open AccessArticle

Star-Shaped Fe_3-xO₄-Au Core-Shell Nanoparticles: From Synthesis to SERS Application

by Thi Thuy Nguyen, Stephanie Lau-Truong, Fayna Mammeri and Souad Ammar

Nanomaterials 2020, 10(2), 294; https://doi.org/10.3390/nano10020294 - 10 Feb 2020

Cited by 16 | Viewed by 3466

Abstract

In this work, the preparation of magneto-plasmonic granular nanostructures and their evaluation as efficient substrates for magnetically assisted surface enhanced Raman spectroscopy (SERS) sensing are discussed. These nanostructures consist of star-shaped gold Au shell grown on iron oxide Fe_3-xO₄ multicores. They were prepared by seed-mediated growth of anisotropic, in shape gold nanosatellites attached to the surface of polyol-made iron oxide polycrystals. In practice, the 180 nm-sized spherical iron oxide particles were functionalized by (3-aminopropyl) triethoxysilane (APTES) to become positively charged and to interact, in solution, with negatively charged 2 nm-sized Au single crystals, leading to nanohybrids. These hybrids acted subsequently as nucleation platforms for the growth of a branched gold shell, when they were contacted to a fresh HAuCl₄ gold salt aqueous solution, in the presence of hydroquinone, a reducing agent, for an optimized nominal weight ratio between both the starting hybrids and the gold salt. As expected, the resulting nanocomposites exhibit a high saturation magnetization at room temperature and a rough enough plasmonic surface, making them easily attracted by a lab. magnet, while exhibiting a great number of SERS hot spots. Preliminary SERS detection assays were successfully performed on diluted aqueous thiram solution (10⁻⁸ M), using these engineered substrates, highlighting their capability to be used as chemical trace sensors. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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15 pages, 7106 KiB

Open AccessArticle

Ecotoxicological Studies of ZnO and CdS Nanoparticles on Chlorella vulgaris Photosynthetic Microorganism in Seine River Water

by Alice da Rocha, Nicolas Menguy, Claude Yéprémian, Alain Couté and Roberta Brayner

Nanomaterials 2020, 10(2), 227; https://doi.org/10.3390/nano10020227 - 28 Jan 2020

Cited by 5 | Viewed by 2344

Abstract

Seine river water was used as natural environmental medium to study the ecotoxicological impact of ZnO and CdS nanoparticles and Zn²⁺ and Cd²⁺ free ions using Chlorella vulgaris as a biological target. It was demonstrated by viability tests and photosynthetic activity measurements that free Zn²⁺ (IC₅₀ = 2.7 × 10⁻⁴ M) is less toxic than free Cd²⁺ and ZnO nanoparticles (IC₅₀ = 1.4 × 10⁻⁴ M). In the case of cadmium species, free Cd²⁺ (IC₅₀ = 3.5 × 10⁻⁵ M) was similar to CdS nanoparticles (CdS-1: IC₅₀ = 1.9 × 10⁻⁵ M and CdS-2: IC₅₀ = 1.9 × 10⁻⁵ M), as follows: CdS > Cd²⁺ > ZnO > Zn²⁺. Adenosine-5’-triphosphate (ATP) assay and superoxide dismutase (SOD) enzymatic activity confirmed these results. Transmission electron microscopy (TEM), coupled with energy-dispersive X-ray spectroscopy (EDS), confirmed the internalization of CdS-1 nanoparticles after 48 h of contact with Chlorella vulgaris at 10⁻³ M. With a higher concentration of nanoparticles (10⁻² M), ZnO and CdS-2 were also localized inside cells. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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11 pages, 2903 KiB

Open AccessCommunication

Polyol Process Coupled to Cold Plasma as a New and Efficient Nanohydride Processing Method: Nano-Ni₂H as a Case Study

by Sonia Haj-Khlifa, Sophie Nowak, Patricia Beaunier, Patricia De Rango, Michaël Redolfi and Souad Ammar-Merah

Nanomaterials 2020, 10(1), 136; https://doi.org/10.3390/nano10010136 - 12 Jan 2020

Cited by 4 | Viewed by 2692 | Correction

Abstract

An alternative route for metal hydrogenation has been investigated: cold plasma hydrogen implantation on polyol-made transition metal nanoparticles. This treatment applied to a challenging system, Ni–H, induces a re-ordering of the metal lattice, and superstructure lines have been observed by both Bragg–Brentano and grazing incidence X-ray diffraction. The resulting intermetallic structure is similar to those obtained by very high-pressure hydrogenation of nickel and prompt us to suggest that plasma-based hydrogen implantation in nanometals is likely to generate unusual metal hydride, opening new opportunities in chemisorption hydrogen storage. Typically, almost isotropic in shape and about 30 nm sized hexagonal-packed Ni₂H single crystals were produced starting from similarly sized cubic face-centred Ni polycrystals. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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17 pages, 6427 KiB

Open AccessArticle

Ascorbic Acid-Assisted Polyol Synthesis of Iron and Fe/GO, Fe/h-BN Composites for Pb²⁺ Removal from Wastewaters

by Denis Leybo, Marat Tagirov, Elizaveta Permyakova, Anton Konopatsky, Konstantin Firestein, Feruza Tuyakova, Dmitry Arkhipov and Denis Kuznetsov

Nanomaterials 2020, 10(1), 37; https://doi.org/10.3390/nano10010037 - 22 Dec 2019

Cited by 10 | Viewed by 2670

Abstract

Iron powders and Fe/graphene oxide and Fe/boron nitride composites were synthesized by means of a polyol synthesis method. The effect of NaOH/Fe and ascorbic acid/Fe ratios on the characteristics of synthesized products were evaluated. The samples were characterized by X-ray diffraction, scanning and transmission electron microscopy, low-temperature nitrogen adsorption and Raman-spectroscopy. Ascorbic acid-assisted polyol synthesis resulted in the 10-fold decrease of the iron particles’ size and almost 2-fold increase of lead removal efficiency. The deposition of iron on the surface of graphene oxide lead to the formation of small 20–30 nm sized particles as well as bigger 200–300 nm sized particles, while the reduction in presence of boron nitride resulted in the 100–200 nm sized particles. The difference is attributed to the surface state of graphene oxide and boron nitride. Adsorption properties of the obtained materials were studied in the process of Pb²⁺ ion removal from wastewater. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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16 pages, 7412 KiB

Open AccessArticle

Investigation of Polyol Process for the Synthesis of Highly Pure BiFeO₃ Ovoid-Like Shape Nanostructured Powders

by Manel Missaoui, Sandrine Coste, Maud Barré, Anthony Rousseau, Yaovi Gagou, Mohamed Ellouze and Nirina Randrianantoandro

Nanomaterials 2020, 10(1), 26; https://doi.org/10.3390/nano10010026 - 20 Dec 2019

Cited by 4 | Viewed by 2417

Abstract

Exclusive and unprecedented interest was accorded in this paper to the synthesis of BiFeO₃ nanopowders by the polyol process. The synthesis protocol was explored and adjusted to control the purity and the grain size of the final product. The optimum parameters were carefully established and an average crystallite size of about 40 nm was obtained. XRD and Mössbauer measurements proved the high purity of the synthesized nanostructurated powders and confirmed the persistence of the rhombohedral R3c symmetry. The first studies on the magnetic properties show a noticeable widening of the hysteresis loop despite the remaining cycloidal magnetic structure, promoting the enhancement of the ferromagnetic order and consequently the magnetoelectric coupling compared to micrometric size powders. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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18 pages, 6758 KiB

Open AccessArticle

Nanoparticles (NPs) of WO_3-x Compounds by Polyol Route with Enhanced Photochromic Properties

by Marie Bourdin, Manuel Gaudon, François Weill, Mathieu Duttine, Marion Gayot, Younes Messaddeq and Thierry Cardinal

Nanomaterials 2019, 9(11), 1555; https://doi.org/10.3390/nano9111555 - 01 Nov 2019

Cited by 26 | Viewed by 4444

Abstract

Tungsten trioxide (WO₃) is well-known as one of the most promising chromogenic compounds. It has a drastic change of coloration induced from different external stimuli and so its applications are developed as gas sensors, electrochromic panels or photochromic sensors. This paper focuses on the photochromic properties of nanoWO₃, with tunable composition (with tunable oxygen sub-stoichiometry). Three reference samples with yellow, blue and black colors were prepared from polyol synthesis followed by post annealing under air, none post-annealing treatment, or a post-annealing under argon atmosphere. These three samples differ in terms of crystallographic structure (cubic system versus monoclinic system), oxygen vacancy concentration, electronic band diagram with occurrence of free or trapped electrons and their photochromic behavior. Constituting one main finding, it is shown that the photochromic behavior is highly dependent on the compound’s composition/color. Rapid and important change of coloration under UV (ultraviolet) irradiation was evidenced especially on the blue compound, i.e., the photochromic coloring efficiency of this compound in terms of contrast between bleached and colored phase, as the kinetic aspect is high. The photochromism is reversible in a few hours. This hence opens a new window for the use of tungsten oxide as smart photochromic compounds. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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11 pages, 15669 KiB

Open AccessArticle

Polyol-Mediated Synthesis of Nitrogen-Containing Carbon-Dots from Tetracyanobenzene with Intense Red Fluorescence

by Roman Lehmacher and Claus Feldmann

Nanomaterials 2019, 9(10), 1470; https://doi.org/10.3390/nano9101470 - 16 Oct 2019

Cited by 3 | Viewed by 3038

Abstract

Nitrogen-containing C-dots were prepared by heating (160 °C, 1 h) 1,2,4,5-tetracyanobenzene (TCB) in polyethylene glycol 400 (PEG400). The as-prepared monocrystalline C-dots were 2–4 nm in diameter and contained 24.4 wt. % of nitrogen. They showed intense fluorescence under excitation at 400–500 nm as well as under excitation at 600–700 nm. In addition to an excitation-wavelength-depending emission at 400 to 650 nm, the emission spectra exhibited a strong emission peaking at 715 nm, whose position was independent from the wavelength of excitation. For this deep-red emission a remarkable quantum yield of 69% was detected. The synthesis of nitrogen-containing C-dotswas completely performed in the liquid phase. Moreover, the C-dots could be directly dispersed in water. The resulting aqueous suspensions of PEG400-stabilized nitrogen-containing C-dots also showed intense red emission that was visible to the naked eye. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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13 pages, 4416 KiB

Open AccessArticle

Luminescence and X-ray Absorption Properties of Uniform Eu³⁺:(H₃O)Lu₃F₁₀ Nanoprobes

by Daniel González-Mancebo, Ana Isabel Becerro, Ariadna Corral, Marcin Balcerzyk and Manuel Ocaña

Nanomaterials 2019, 9(8), 1153; https://doi.org/10.3390/nano9081153 - 12 Aug 2019

Cited by 4 | Viewed by 2979

Abstract

Due to the high atomic number of lutetium and the low phonon energy of the fluoride matrix, Lu-based fluoride nanoparticles doped with active lanthanide ions are potential candidates as bioprobes in both X-ray computed tomography and luminescent imaging. This paper shows a method for the fabrication of uniform, water-dispersible Eu³⁺:(H₃O)Lu₃F₁₀ nanoparticles doped with different Eu contents. Their luminescent properties were studied by means of excitation and emission spectra as well as decay curves. The X-ray attenuation capacity of the phosphor showing the highest emission intensity was subsequently analyzed and compared with a commercial contrast agent. The results indicated that the 10% Eu³⁺-doped (H₃O)Lu₃F₁₀ nanoparticles fabricated with the proposed polyol-based method are good candidates to be used as dual probes for luminescent imaging and X-ray computed tomography. Full article

(This article belongs to the Special Issue Polyol Synthesis: A Versatile Wet-Chemistry Route for the Design and Production of Functional Inorganic Nanoparticles)

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