scholarly journals Ferrocene Introduced into 5-Methylresorcinol-Based Organic Aerogels

Polymers ◽  
2020 ◽  
Vol 12 (7) ◽  
pp. 1582 ◽  
Author(s):  
Ludmila V. Erkhova ◽  
Igor A. Presniakov ◽  
Michail I. Afanasov ◽  
Dmitry A. Lemenovskiy ◽  
Haojie Yu ◽  
...  

The polycondensation sol–gel reaction of 5-methylresocinol and formaldehyde with additional compounds in reaction media is a relatively simple way to produce modified aerogels. In order to obtain aerogels with a large surface area and high porosity, the conditions for gel formation, the solvent exchange process before drying, and the supercritical drying process were optimized. A successful attempt was made to introduce ferrocene units into 5-methylresocinol-formaldehyde-based aerogels. The resulting aerogels are amorphous substrates, and no aggregated ferrocene units were found in their structures. All of the aerogel samples that were obtained are structurally similar despite differences in the original ferrocene units and their initial concentration. It was found that the inclusion limit of ferrocene structural blocks into an aerogel is ~6% wt. The structures of the inclusions in which all of the Fe atoms in the aerogel substrates were present in ferrocene/ferrocenium at an approximate ratio of 60/40 to 55/45 were confirmed by X-ray photoelectron spectroscopy and Mössbauer spectroscopy. Aerogels with ferrocene/ferrocenium inclusions are likely to exhibit reversible redox activity in reactions with gaseous reagents.

2011 ◽  
Vol 1306 ◽  
Author(s):  
Anja Veronovski ◽  
Zoran Novak ◽  
Knez Željko

ABSTRACTThere are a lot of synthetic polymers which can be used for controlled drug delivery, however they are not easily accepted by the organism. Also incorporation of drugs into carriers runs under difficult conditions. Therefore scientists have been inclined to use natural-origin polymers, such as proteins and polysaccharides. Some of these promising natural polysaccharidic candidates are alginic acid sodium salt, guar gum and chitosan due to their outstanding merits. They are similar to extracellular matrix having high chemical versatility, good biological performance and cell or enzyme-controlled degradability. Many polysaccharidic hydrogels for drug delivery have already been prepared, but one of their weakness is their short life in dry air conditions; thus, special coating materials are being developed for enhancing their life time.Alginates were used in the present research for synthesis of organic biodegradable gels by sol-gel process, which were further easily converted to aerogels by supercritical drying. They are safe for use, nontoxic, and derived from renewable sources. Aerogels made of alginate are dry and stable materials, which makes them interesting as a substitute to hydrogels. Alginates undergo reversible gelation in aqueous solution through interaction with divalent cations such as Ca2+, which create ionic inter-chain bridges. Two fundamental methods of ionic cross-linking were used to prepare alginate hydrogels: the diffusion method, where spheres are created and the internal setting method resulting in monoliths. After producing the hydrogel, alcogels were formed by solvent exchange using 100% ethanol. Ethanol was later replaced by supercritical CO2 with supercritical drying (100 bar, 35°C). Aerogels made from natural polysaccharides combine both biocharacteristics and aerogel characteristics such as high porosity and specific surface area, which makes them really attractive in drug delivery applications. The aerogels obtained in present research were therefore studied as drug carriers. The effects of the alginate composition and synthesis method on model drug nicotinic acid release were investigated. The results indicated that by using the internal setting cross-linking method for obtaining aerogels nicotinic acid was released in a more controlled manner. That is why further investigation was done on alginate spherical beads for prolonging their drug release. A multi-step sol-gel process was applied to generate complex aerogels with multi-membranes. First ionically cross-linked spherical cores were obtained by dropwise addition of sodium alginate solution into a CaCl2 solution. These cores were further immersed into alginate solution, filtered through a sieve and dropped into a salt solution again. By repeating the above process, different multi-membrane hydrogels were produced and further converted to aerogels. By adding more membranes around core burst drug release was successfully inhibited.


Author(s):  
G.C. Ruben ◽  
R.W. Pekala

The sol-gel polymerization of metal alkoxides or certain multifunctional organic monomers leads to the formation of highly crosslinked, transparent gels. If the solvent is simply evaporated from the pores of these gels, large capillary forces are exerted, and a collapsed structure known as a xerogel is formed. In order to preserve the gel skeleton, it is necessary to remove the the aforementioned solvent under supercritical conditions. The low density, microporous material that results from this operation is known as an aerogel. Aerogels have an ultrafine cell/pore size (< 500 Å), connected porosity, high surface areas (400-1000 m2/g), and an ultrastructure composed of interconnected colloidal-like particles or polymeric chains with characteristic dimensions of 100 Å. This ultrastructure is responsible for the unique optical, thermal, and acoustic properties of aerogels. For example, the ultrafine cell/pore size minimizes light scattering; and thus, aerogels are transparent porous solids. The high porosity of aerogels makes them excellent insulators with their thermal conductivity being approximately 100X lower than that of the fully dense matrix. Finally, the aerogel skeleton is responsible for the low sound velocities observed in these materials (i.e. 100-300 m/sec).


MRS Bulletin ◽  
1990 ◽  
Vol 15 (12) ◽  
pp. 30-36

Aerogels are a special class of open-cell foams derived from the supercritical drying of highly cross-linked inorganic or organic gels. These materials have ultrafine cell/pore sizes (less than 1,000 Å), continuous porosity, high surface area (400–1000 m2/g), and a microstructure composed of interconnected colloidal-like particles or polymeric chains with characteristic diameters of 100 Å. This microstructure is responsible for the unusual optical, acoustic, thermal, and mechanical properties of aerogels. For example, aerogels can be prepared as transparent, porous solids because their ultrafine cell/pore size minimizes light scattering in the visible spectrum. Figure 4.1 shows the different aerogels that will be discussed in this article.The hydrolysis and condensation of metal alkoxides is the most common synthetic route for the formation of inorganic aerogels. Inorganic aerogels have been prepared from monomers such as tetraisopropoxy titanate, aluminum secbutylate, and zirconium isopropoxide. Nevertheless, the majority of scientific research has concentrated on the sol-gel polymerization of tetramethoxysilane (TMOS), or the less toxic tetraethoxysilane (TEOS). The resultant silica aerogels are being investigated for applications ranging from window insulation to the collection of hypervelocity partis cles in space.The sol-gel polymerization of a multifunctional monomer in solution, leading to the formation of an aerogel, is not unique to metal alkoxides. Organic reactions that proceed through a sol-gel transition have been discovered recently.


2010 ◽  
Vol 148-149 ◽  
pp. 920-923
Author(s):  
Yue Qing Zhao ◽  
Ying Hua Liang ◽  
Feng Feng Li ◽  
Hong Ping Chen ◽  
Xin Hua Liu ◽  
...  

CuO-CoO-MnO/SiO2 nanocomposite aerogels were prepared by using tetraethyl orthosilicate (TEOS) as Si source, and aqueous solution of Cu, Co and Mn acetates as transition metal sources via sol-gel process and supercritical drying (SCD) technique. The effect of synthesis conditions on gelation was investigated. The composition of the nanocomposite aerogels was characterized by electron dispersive spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS). The specific surface area of the nanocomposite aerogels was determined by the Brunauer-Emmett-Teller (BET) method. The results show that the range of optimal temperature for gelation is 30-45 °C, and the pH is 3.0-4.5. CuO-CoO-MnO/SiO2 nanocomposite aerogels are porous with a specific surface area of 384.9-700.6 m2/g. Compared to CO2 SCD, ethanol SCD is even favorable to the formation of aerogel with high specific surface area. The transition metals content in the nanocomposite aerogels can be controlled to be 0.71-13.77 at.%.


2019 ◽  
Author(s):  
Georg Dewald ◽  
Saneyuki Ohno ◽  
Marvin Kraft ◽  
Raimund Koerver ◽  
Paul Till ◽  
...  

<p>All-solid-state batteries are often expected to replace conventional lithium-ion batteries in the future. However, the practical electrochemical and cycling stability of the best-conducting solid electrolytes, i.e. lithium thiophosphates, are still critical issues that prevent long-term stable high-energy cells. In this study, we use <i>stepwise</i><i>cyclic voltammetry </i>to obtain information on the practical oxidative stability limit of Li<sub>10</sub>GeP<sub>2</sub>S<sub>12</sub>, a Li<sub>2</sub>S‑P<sub>2</sub>S<sub>5</sub>glass, as well as the argyrodite Li<sub>6</sub>PS<sub>5</sub>Cl solid electrolytes. We employ indium metal and carbon black as the counter and working electrode, respectively, the latter to increase the interfacial contact area to the electrolyte as compared to the commonly used planar steel electrodes. Using a stepwise increase in the reversal potentials, the onset potential at 25 °C of oxidative decomposition at the electrode-electrolyte interface is identified. X‑ray photoelectron spectroscopy is used to investigate the oxidation of sulfur(-II) in the thiophosphate polyanions to sulfur(0) as the dominant redox process in all electrolytes tested. Our results suggest that after the formation of these decomposition products, significant redox behavior is observed. This explains previously reported redox activity of thiophosphate solid electrolytes, which contributes to the overall cell performance in solid-state batteries. The <i>stepwise cyclic voltammetry</i>approach presented here shows that the practical oxidative stability at 25 °C of thiophosphate solid electrolytes against carbon is kinetically higher than predicted by thermodynamic calculations. The method serves as an efficient guideline for the determination of practical, kinetic stability limits of solid electrolytes. </p>


2019 ◽  
Author(s):  
Georg Dewald ◽  
Saneyuki Ohno ◽  
Marvin Kraft ◽  
Raimund Koerver ◽  
Paul Till ◽  
...  

<p>All-solid-state batteries are often expected to replace conventional lithium-ion batteries in the future. However, the practical electrochemical and cycling stability of the best-conducting solid electrolytes, i.e. lithium thiophosphates, are still critical issues that prevent long-term stable high-energy cells. In this study, we use <i>stepwise</i><i>cyclic voltammetry </i>to obtain information on the practical oxidative stability limit of Li<sub>10</sub>GeP<sub>2</sub>S<sub>12</sub>, a Li<sub>2</sub>S‑P<sub>2</sub>S<sub>5</sub>glass, as well as the argyrodite Li<sub>6</sub>PS<sub>5</sub>Cl solid electrolytes. We employ indium metal and carbon black as the counter and working electrode, respectively, the latter to increase the interfacial contact area to the electrolyte as compared to the commonly used planar steel electrodes. Using a stepwise increase in the reversal potentials, the onset potential at 25 °C of oxidative decomposition at the electrode-electrolyte interface is identified. X‑ray photoelectron spectroscopy is used to investigate the oxidation of sulfur(-II) in the thiophosphate polyanions to sulfur(0) as the dominant redox process in all electrolytes tested. Our results suggest that after the formation of these decomposition products, significant redox behavior is observed. This explains previously reported redox activity of thiophosphate solid electrolytes, which contributes to the overall cell performance in solid-state batteries. The <i>stepwise cyclic voltammetry</i>approach presented here shows that the practical oxidative stability at 25 °C of thiophosphate solid electrolytes against carbon is kinetically higher than predicted by thermodynamic calculations. The method serves as an efficient guideline for the determination of practical, kinetic stability limits of solid electrolytes. </p>


Nanomaterials ◽  
2021 ◽  
Vol 11 (7) ◽  
pp. 1738
Author(s):  
Saeid Vafaei ◽  
Alexander Wolosz ◽  
Catlin Ethridge ◽  
Udo Schnupf ◽  
Nagisa Hattori ◽  
...  

SnO2 nanoparticles are regarded as attractive, functional materials because of their versatile applications. SnO2 nanoaggregates with single-nanometer-scale lumpy surfaces provide opportunities to enhance hetero-material interfacial areas, leading to the performance improvement of materials and devices. For the first time, we demonstrate that SnO2 nanoaggregates with oxygen vacancies can be produced by a simple, low-temperature sol-gel approach combined with freeze-drying. We characterize the initiation of the low-temperature crystal growth of the obtained SnO2 nanoaggregates using high-resolution transmission electron microscopy (HRTEM). The results indicate that Sn (II) hydroxide precursors are converted into submicrometer-scale nanoaggregates consisting of uniform SnO2 spherical nanocrystals (2~5 nm in size). As the sol-gel reaction time increases, further crystallization is observed through the neighboring particles in a confined part of the aggregates, while the specific surface areas of the SnO2 samples increase concomitantly. In addition, X-ray photoelectron spectroscopy (XPS) measurements suggest that Sn (II) ions exist in the SnO2 samples when the reactions are stopped after a short time or when a relatively high concentration of Sn (II) is involved in the corresponding sol-gel reactions. Understanding this low-temperature growth of 3D SnO2 will provide new avenues for developing and producing high-performance, photofunctional nanomaterials via a cost-effective and scalable method.


Separations ◽  
2021 ◽  
Vol 8 (3) ◽  
pp. 25
Author(s):  
Chukwuka Bethel Anucha ◽  
Ilknur Altin ◽  
Emin Bacaksız ◽  
Tayfur Kucukomeroglu ◽  
Masho Hilawie Belay ◽  
...  

Abatement of contaminants of emerging concerns (CECs) in water sources has been widely studied employing TiO2 based heterogeneous photocatalysis. However, low quantum energy yield among other limitations of titania has led to its modification with other semiconductor materials for improved photocatalytic activity. In this work, a 0.05 wt.% CuWO4 over TiO2 was prepared as a powder composite. Each component part synthesized via the sol-gel method for TiO2, and CuWO4 by co-precipitation assisted hydrothermal method from precursor salts, underwent gentle mechanical agitation. Homogenization of the nanopowder precursors was performed by zirconia ball milling for 2 h. The final material was obtained after annealing at 500 °C for 3.5 h. Structural and morphological characterization of the synthesized material has been achieved employing X-ray diffraction (XRD), Fourier transform infra-red (FTIR) spectroscopy, Brunauer–Emmett–Teller (BET) N2 adsorption–desorption analysis, Scanning electron microscopy-coupled Energy dispersive X-ray spectroscopy (SEM-EDS), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), and UV-Vis diffuse reflectance spectroscopy (UV-vis DRS) for optical characterization. The 0.05 wt.% CuWO4-TiO2 catalyst was investigated for its photocatalytic activity over carbamazepine (CBZ), achieving a degradation of almost 100% after 2 h irradiation. A comparison with pure TiO2 prepared under those same conditions was made. The effect of pH, chemical scavengers, H2O2 as well as contaminant ion effects (anions, cations), and humic acid (HA) was investigated, and their related influences on the photocatalyst efficiency towards CBZ degradation highlighted accordingly.


2021 ◽  
Vol 3 (7) ◽  
Author(s):  
Alexandre Pancotti ◽  
Dener Pereira Santos ◽  
Dielly Oliveira Morais ◽  
Mauro Vinícius de Barros Souza ◽  
Débora R. Lima ◽  
...  

AbstractIn this study, we report the synthesis and characterization of NiFe2O4 and CoFe2O4 nanoparticles (NPs) which are widely used in the biomedical area. There is still limited knowledge how the properties of these materials are influenced by different chemical routes. In this work, we investigated the effect of heat treatment over cytotoxicity of cobalt and niquel ferrites NPs synthesized by sol-gel method. Then the samples were studied using transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), vibrating sample magnetometer (VSM), Fourier Transform Infrared Spectroscopy Analysis (FTIR), and X-ray fluorescence (XRF). The average crystallite sizes of the particles were found to be in the range of 20–35 nm. The hemocompatibility (erythrocytes and leukocytes) was checked. Cytotoxicity results were similar to those of the control test sample, therefore suggesting hemocompatibility of the tested materials.


Electronics ◽  
2021 ◽  
Vol 10 (9) ◽  
pp. 1099
Author(s):  
Ye-Ji Han ◽  
Se Hyeong Lee ◽  
So-Young Bak ◽  
Tae-Hee Han ◽  
Sangwoo Kim ◽  
...  

Conventional sol-gel solutions have received significant attention in thin-film transistor (TFT) manufacturing because of their advantages such as simple processing, large-scale applicability, and low cost. However, conventional sol-gel processed zinc tin oxide (ZTO) TFTs have a thermal limitation in that they require high annealing temperatures of more than 500 °C, which are incompatible with most flexible plastic substrates. In this study, to overcome the thermal limitation of conventional sol-gel processed ZTO TFTs, we demonstrated a ZTO TFT that was fabricated at low annealing temperatures of 350 °C using self-combustion. The optimized device exhibited satisfactory performance, with μsat of 4.72 cm2/V∙s, Vth of −1.28 V, SS of 0.86 V/decade, and ION/OFF of 1.70 × 106 at a low annealing temperature of 350 °C for one hour. To compare a conventional sol-gel processed ZTO TFT with the optimized device, thermogravimetric and differential thermal analyses (TG-DTA) and X-ray photoelectron spectroscopy (XPS) were implemented.


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