Special Issue "Sol-Gel Preparation of Nanomaterials"

A special issue of Nanomaterials (ISSN 2079-4991).

Deadline for manuscript submissions: 15 December 2018

Special Issue Editor

Guest Editor
Prof. Dr. Erhard Kemnitz

Full University Professor, Chemistry Department, Humboldt-Universität zu Berlin, Brook-Taylor-Str. 2, D-12489 Berlin, Germany
Website | E-Mail
Interests: mechanistic aspects of heterogeneously catalysed fluorination reactions, non-aqueous fluorolytic sol–gel synthesis of nanoscopic metal fluorides; nano metal fluorides as solid Lewis acids; nano metal hydroxide fluorides as biacidic Brønsted/Lewis acids and bases; metal fluoride sols for antireflective coating; inorganic–organic hybrid materials based on nano metal fluorides

Special Issue Information

Dear Colleagues,

Nanomaterial chemistry has become an extremely important area of research over the past 20 years. Although many different nanomaterials have already found industrial applications we are still just at the beginning of a new scientific and industrial revolution driven by the advances in nanomaterials science.

Over the past decades, many new synthesis techniques have been developed that give access to the fascinating world of nanomaterials with different chemical and physical properties. The sol-gel synthesis certainly is one of the most powerful synthesis routes in terms of the wide variety of synthesis approaches and technical applications. Especially the classical (aqueous) sol-gel synthesis route, mainly forced by the development of silica, was but still is in the focus of thousands of chemists and materials scientists worldwide.

However, motivated by new developments like atomic layer deposition, ALD, and others, non-aqueous sol-gel synthesis approaches have been developed recently, thus extending the synthesis access toward nanoscopic new materials.

Therefore, it is the intention of the Special Issue of Nanomaterials to present the current state-of-the-art in the sol-gel-based synthesis approaches towards nanomaterials. Characteristic properties and fields of applications of those materials may highlight the potential of these synthesis approaches. On a first glance, there is no restriction on classes of sol-gel formed nanomaterials as well as field of application. Therefore, in the present Special Issue, contributions from leading groups in the field with the aim of giving a balanced view of the current state-of-the-art in the sol-gel-synthesis field are invited.

Prof. Dr. Erhard Kemnitz
Guest Editor

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Keywords

  • Sol-Gel Synthesis
  • Nanomaterials
  • Nanotechnology
  • Mechanistic Synthesis Aspects
  • Properties
  • Applications

Published Papers (7 papers)

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Research

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Open AccessArticle Non-Aqueous Sol-Gel Synthesis of FePt Nanoparticles in the Absence of In Situ Stabilizers
Nanomaterials 2018, 8(5), 297; https://doi.org/10.3390/nano8050297
Received: 31 March 2018 / Revised: 24 April 2018 / Accepted: 30 April 2018 / Published: 3 May 2018
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Abstract
The synthesis of FePt nanocrystals is typically performed in an organic solvent at rather high temperatures, demanding the addition of the in situ stabilizers oleic acid and oleylamine to produce monomodal particles with well-defined morphologies. Replacing frequently-used solvents with organic media bearing functional
[...] Read more.
The synthesis of FePt nanocrystals is typically performed in an organic solvent at rather high temperatures, demanding the addition of the in situ stabilizers oleic acid and oleylamine to produce monomodal particles with well-defined morphologies. Replacing frequently-used solvents with organic media bearing functional moieties, the use of the stabilizers can be completely circumvented. In addition, various morphologies and sizes of the nanocrystals can be achieved by the choice of organic solvent. The kinetics of particle growth and the change in the magnetic behavior of the superparamagnetic FePt nanocrystals during the synthesis with a set of different solvents, as well as the resulting morphologies and stoichiometries of the nanoparticles were determined by powder X-ray diffraction (PXRD), small-angle X-ray scattering (SAXS), transmission electron microscopy (TEM), inductively coupled plasma optical emission spectroscopy (ICP-OES)/mass spectrometry (ICP-MS), and superconducting quantum interference device (SQUID) measurements. Furthermore, annealing of the as-prepared FePt nanoparticles led to the ordered L10 phase and, thus, to hard magnetic materials with varying saturation magnetizations and magnetic coercivities. Full article
(This article belongs to the Special Issue Sol-Gel Preparation of Nanomaterials)
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Open AccessArticle Cobalt-Assisted Morphology and Assembly Control of Co-Doped ZnO Nanoparticles
Nanomaterials 2018, 8(4), 249; https://doi.org/10.3390/nano8040249
Received: 20 March 2018 / Revised: 13 April 2018 / Accepted: 14 April 2018 / Published: 17 April 2018
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Abstract
The morphology of metal oxide nanostructures influences the response of the materials in a given application. In addition to changing the composition, doping can also modify the morphology of a host nanomaterial. Herein, we determine the effect of dopant concentration, reaction temperature, and
[...] Read more.
The morphology of metal oxide nanostructures influences the response of the materials in a given application. In addition to changing the composition, doping can also modify the morphology of a host nanomaterial. Herein, we determine the effect of dopant concentration, reaction temperature, and reaction time on the morphology and assembly of CoxZn1−xO nanoparticles synthesized through non-aqueous sol-gel in benzyl alcohol. With the increase of the atom % of cobalt incorporated from 0 to 15, the shape of the nanoparticles changes from near spherical, to irregular, and finally to triangular. The tendency of the particles to assemble increases in the same direction, with Co0.05Zn0.95O consisting of non-assembled particles, whereas Co0.15Zn0.85O consists of triangular nanoparticles forming spherical structures. The morphology and assembly process are also sensitive to the reaction temperature. The assembly process is found to occur during the nucleation or the early stages of particle growth. The cobalt ions promote the change in the shape during the growth stage of the nanoparticles. Full article
(This article belongs to the Special Issue Sol-Gel Preparation of Nanomaterials)
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Open AccessArticle The Effect of Different Coupling Agents on Nano-ZnO Materials Obtained via the Sol–Gel Process
Nanomaterials 2017, 7(12), 439; https://doi.org/10.3390/nano7120439
Received: 10 October 2017 / Revised: 27 November 2017 / Accepted: 8 December 2017 / Published: 12 December 2017
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Abstract
Hybrid nanomaterials based on zinc oxide were synthesized via the sol–gel method, using different silane coupling agents: (3-glycidyloxypropyl)trimethoxysilane (GPTMS), phenyltriethoxysilane (PhTES), octyltriethoxysilane (OTES), and octadecyltriethoxysilane (ODTES). Morphological properties and the silane precursor type effect on the particle size were investigated using dynamic light
[...] Read more.
Hybrid nanomaterials based on zinc oxide were synthesized via the sol–gel method, using different silane coupling agents: (3-glycidyloxypropyl)trimethoxysilane (GPTMS), phenyltriethoxysilane (PhTES), octyltriethoxysilane (OTES), and octadecyltriethoxysilane (ODTES). Morphological properties and the silane precursor type effect on the particle size were investigated using dynamic light scattering (DLS), environmental scanning electron microscopy (ESEM), transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and X-ray diffraction (XRD). The bonding characteristics of modified ZnO materials were investigated using Fourier transform infrared spectroscopy (FTIR). The final solutions were deposited on metallic substrate (aluminum) in order to realize coatings with various wettability and roughness. The morphological studies, obtained by ESEM and TEM analysis, showed that the sizes of the ZnO nanoparticles are changed as function of silane precursor used in synthesis. The thermal stability of modified ZnO materials showed that the degradation of the alkyl groups takes place in the 300–500 °C range. Water wettability study revealed a contact angle of 142 ± 5° for the surface covered with ZnO material modified with ODTES and showed that the water contact angle increases as the alkyl chain from the silica precursor increases. These modified ZnO materials, therefore, can be easily incorporated in coatings for various applications such as anti-corrosion and anti-icing. Full article
(This article belongs to the Special Issue Sol-Gel Preparation of Nanomaterials)
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Open AccessFeature PaperArticle Sol-Gel-Synthesis of Nanoscopic Complex Metal Fluorides
Nanomaterials 2017, 7(11), 362; https://doi.org/10.3390/nano7110362
Received: 14 September 2017 / Revised: 17 October 2017 / Accepted: 24 October 2017 / Published: 2 November 2017
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Abstract
The fluorolytic sol-gel synthesis for binary metal fluorides (AlF3, CaF2, MgF2) has been extended to ternary and quaternary alkaline earth metal fluorides (CaAlF5, Ca2AlF7, LiMgAlF6). The formation and crystallization
[...] Read more.
The fluorolytic sol-gel synthesis for binary metal fluorides (AlF3, CaF2, MgF2) has been extended to ternary and quaternary alkaline earth metal fluorides (CaAlF5, Ca2AlF7, LiMgAlF6). The formation and crystallization of nanoscopic ternary CaAlF5 and Ca2AlF7 sols in ethanol were studied by 19F liquid and solid state NMR (nuclear magnetic resonance) spectroscopy, as well as transmission electron microscopy (TEM). The crystalline phases of the annealed CaAlF5, Ca2AlF7, and LiMgAlF6 xerogels between 500 and 700 °C could be determined by X-ray powder diffraction (XRD) and 19F solid state NMR spectroscopy. The thermal behavior of un-annealed nanoscopic ternary and quaternary metal fluoride xerogels was ascertained by thermal analysis (TG/DTA). The obtained crystalline phases of CaAlF5 and Ca2AlF7 derived from non-aqueous sol-gel process were compared to crystalline phases from the literature. The corresponding nanoscopic complex metal fluoride could provide a new approach in ceramic and luminescence applications. Full article
(This article belongs to the Special Issue Sol-Gel Preparation of Nanomaterials)
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Open AccessFeature PaperArticle Sol-Gel Derived Adsorbents with Enzymatic and Complexonate Functions for Complex Water Remediation
Nanomaterials 2017, 7(10), 298; https://doi.org/10.3390/nano7100298
Received: 30 August 2017 / Revised: 18 September 2017 / Accepted: 19 September 2017 / Published: 28 September 2017
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Abstract
Sol-gel technology is a versatile tool for preparation of complex silica-based materials with targeting functions for use as adsorbents in water purification. Most efficient removal of organic pollutants is achieved by using enzymatic reagents grafted on nano-carriers. However, enzymes are easily deactivated in
[...] Read more.
Sol-gel technology is a versatile tool for preparation of complex silica-based materials with targeting functions for use as adsorbents in water purification. Most efficient removal of organic pollutants is achieved by using enzymatic reagents grafted on nano-carriers. However, enzymes are easily deactivated in the presence of heavy metal cations. In this work, we avoided inactivation of immobilized urease by Cu (II) and Cd (II) ions using magnetic nanoparticles provided with additional complexonate (diethylene triamine pentaacetic acid or DTPA) functions. Obtained nanomaterials were characterized by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), and scanning electron microscopy (SEM). According to TGA, the obtained Fe3O4/SiO2-NH2-DTPA nanoadsorbents contained up to 0.401 mmol/g of DTPA groups. In the concentration range Ceq = 0–50 mmol/L, maximum adsorption capacities towards Cu (II) and Cd (II) ions were 1.1 mmol/g and 1.7 mmol/g, respectively. Langmuir adsorption model fits experimental data in concentration range Ceq = 0–10 mmol/L. The adsorption mechanisms have been evaluated for both of cations. Crosslinking of 5 wt % of immobilized urease with glutaraldehyde prevented the loss of the enzyme in repeated use of the adsorbent and improved the stability of the enzymatic function leading to unchanged activity in at least 18 cycles. Crosslinking of 10 wt % urease on the surface of the particles allowed a decrease in urea concentration in 20 mmol/L model solutions to 2 mmol/L in up to 10 consequent decomposition cycles. Due to the presence of DTPA groups, Cu2+ ions in concentration 1 µmol/L did not significantly affect the urease activity. Obtained magnetic Fe3O4/SiO2-NH2-DTPA-Urease nanocomposite sorbents revealed a high potential for urease decomposition, even in presence of heavy metal ions. Full article
(This article belongs to the Special Issue Sol-Gel Preparation of Nanomaterials)
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Open AccessArticle Thermal Conductivity of a Nanoscale Yttrium Iron Garnet Thin-Film Prepared by the Sol-Gel Process
Nanomaterials 2017, 7(9), 247; https://doi.org/10.3390/nano7090247
Received: 23 July 2017 / Revised: 28 August 2017 / Accepted: 29 August 2017 / Published: 31 August 2017
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Abstract
The thermal conductivity of a nanoscale yttrium iron garnet (Y3Fe5O12, YIG) thin-film prepared by a sol-gel method was evaluated using the ultrafast pump-probe technique in the present study. The thermoreflectance change on the surface of a 250
[...] Read more.
The thermal conductivity of a nanoscale yttrium iron garnet (Y3Fe5O12, YIG) thin-film prepared by a sol-gel method was evaluated using the ultrafast pump-probe technique in the present study. The thermoreflectance change on the surface of a 250 nm thick YIG film, induced by the irradiation of femtosecond laser pulses, was measured, and curve fitting of a numerical solution for the transient heat conduction equation to the experimental data was performed using the finite difference method in order to extract the thermal property. Results show that the film’s thermal conductivity is 22–83% higher than the properties of bulk YIG materials prepared by different fabrication techniques, reflecting the microstructural characteristics and quality of the film. Full article
(This article belongs to the Special Issue Sol-Gel Preparation of Nanomaterials)
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Review

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Open AccessFeature PaperReview Sol-Gel Processing of MgF2 Antireflective Coatings
Nanomaterials 2018, 8(5), 295; https://doi.org/10.3390/nano8050295
Received: 28 March 2018 / Revised: 23 April 2018 / Accepted: 26 April 2018 / Published: 2 May 2018
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Abstract
There are different approaches for the preparation of porous antireflective λ/4 MgF2 films from liquid precursors. Among these, the non-aqueous fluorolytic synthesis of precursor solutions offers many advantages in terms of processing simplicity and scalability. In this paper, the structural features and
[...] Read more.
There are different approaches for the preparation of porous antireflective λ/4 MgF2 films from liquid precursors. Among these, the non-aqueous fluorolytic synthesis of precursor solutions offers many advantages in terms of processing simplicity and scalability. In this paper, the structural features and optical performance of the resulting films are highlighted, and their specific interactions with different inorganic substrates are discussed. Due to their excellent abrasion resistance, coatings have a high potential for applications on glass. Using solvothermal treatment of precursor solutions, also the processing of thermally sensitive polymer substrates becomes feasible. Full article
(This article belongs to the Special Issue Sol-Gel Preparation of Nanomaterials)
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Planned Papers

The below list represents only planned manuscripts. Some of these manuscripts have not been received by the Editorial Office yet. Papers submitted to MDPI journals are subject to peer-review.

Title: Non‐aqueous sol‐gel synthesis of FePt nanoparticles
in absence of in situ stabilizers
Author: Tobias Preller*,†, Dirk Menzel∥, J. Cedric Porsiel†, Bilal Temel†, Georg Garnweitner*,†
Abstract: The synthesis of FePt nanocrystals is typically performed in an organic solvent at comparably high
temperatures, requiring the usage of the in situ stabilizers oleic acid and oleylamine to produce
monomodal particles with well‐defined morphologies. By the replacement of the typically used
solvents by organic media bearing functional moieties, the use of the stabilizer can be omitted.
Furthermore, various morphologies and sizes of the nanocrystals as well as an excess of iron or
platinum atoms at the particle surface can be adjusted by the choice of organic solvent. Thus, the
kinetics of particle growth and the change in the magnetic behavior of the FePt nanocrystals during
the synthesis with the different solvents as well as the resulting morphologies of the nanoparticles
were determined by a variety of analytical methods.

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