scholarly journals Dialkylenecarbonate-Bridged Polysilsesquioxanes: Hybrid Organic-Inorganic Sol-Gels with a Thermally Labile Bridging Group

1999 ◽  
Vol 576 ◽  
Author(s):  
Douglas A. Loy ◽  
James V. Beach ◽  
Brigitta M. Baugher ◽  
Roger A. Assink ◽  
Kenneth J. Shea ◽  
...  
Keyword(s):  
Thermal Treatment ◽  
Functional Groups ◽  
Sol Gel ◽  
Chemical Properties ◽  
Inorganic Materials ◽  
Post Processing ◽  
New Approach ◽  
Bridged Polysilsesquioxane ◽  
Bridging Groups ◽  
Monolithic Xerogels

ABSTRACTIn this paper, we introduce a new approach for altering the properties of bridged polysilsesquioxane xerogels using post-processing modification of the polymeric network. The bridging organic group contains latent functionalities that can be liberated thermally, photochemically, or by chemical means after the gel has been processed to a xerogel. These modifications can produce changes in density, solubility, porosity, and or chemical properties of the material. Since every monomer possesses two latent functional groups, the technique allows for the introduction of high levels of functionality in hybrid organic-inorganic materials. Dialkylenecarbonate-bridged polysilsesquioxane gels were prepared by the sol-gel polymerization of bis(triethoxysilylpropyl)carbonate (1) and bis(triethoxysilylisobutyl)-carbonate (2). Thermal treatment of the resulting non-porous xerogels and aerogels at 300–350°C resulted in quantitative decarboxylation of the dialkylenecarbonate bridging groups to give new hydroxyalkyl and olefinic substituted polysilsesquioxane monolithic xerogels and aerogels that can not be directly prepared through direct sol-gel polymerization of organotrialkoxysilanes.

Nanomaterials, Novel Preparation Routes, and Characterizations

2015 ◽  
pp. 1-40 ◽  
Author(s):  
Irshad A. Wani
Keyword(s):  
Electron Microscopy ◽  
Solid Phase ◽  
Arc Discharge ◽  
Hydrogen Plasma ◽  
Sol Gel ◽  
Chemical Vapour ◽  
Chemical Properties ◽  
Vapour Phase ◽  
Inorganic Materials ◽  
Primary Focus

The important aspect of nanotechnology is the remarkable size dependant physico-chemical properties of nanomaterials that have led to the development of synthesis protocols for synthesizing nanomaterials over a range of sizes, shapes, and chemical compositions. This chapter describes the various aspects of nanotechnology: its dimensions and manipulation of matter with primary focus on inorganic materials. Detailed accounts of various methods lying within top-down and bottom-up synthesis approaches are discussed, like Chemical Vapour Condensation (CVC), arc discharge, hydrogen plasma-metal reaction, and laser pyrolysis in the vapour phase, microemulsion, hydrothermal, sol-gel, sonochemical taking place in the liquid phase, and ball milling carried out in the solid phase. The chapter also presents a brief account of the various characterization techniques used for the identification of the nanomaterials: X-ray diffraction, UV-visible spectroscopy, and electron microscopy (e.g. Transmission Electron Microscopy [TEM], Scanning Electron Microscopy [SEM], Atomic Force Microscopy [AFM]).

scholarly journals Gel Based Sunscreen Containing Surface Modified TiO2Obtained by Sol-Gel Process: Proposal for a Transparent UV Inorganic Filter

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Marina Paiva Abuçafy ◽  
Eloísa Berbel Manaia ◽  
Renata Cristina Kiatkoski Kaminski ◽  
Victor Hugo Sarmento ◽  
Leila Aparecida Chiavacci
Keyword(s):  
Diffuse Reflectance Spectroscopy ◽  
Sol Gel ◽  
Chemical Properties ◽  
High Refractive Index ◽  
Inorganic Materials ◽  
Continuous Exposure ◽  
Sol Gel Process ◽  
Surface Modified ◽  
Physical And Chemical ◽  
Gel Formulations

Inorganic UV filters, as titanium dioxide (TiO2), have become attractive because of their role in protecting the skin against the damage caused by the continuous exposure to the sun. However, their high refractive index, responsible for a white residue when applied on the skin, has led to the development of alternative inorganic materials, such as TiO2nanoparticles. Thus, the aim of this study was the development of transparent and stable gel formulations containing surface modified TiO2nanoparticles for application in sunscreens. Also, the physical and chemical properties of formulations containing TiO2nanoparticles were evaluated. The UV absorption spectroscopy analyses indicated that the formulations containing TiO2nanoparticles had a broad protection spectrum. The diffuse reflectance spectroscopy revealed that the use of PTSH surface modified TiO2nanoparticles improved the transparency of the sunscreen formulations compared to that containing commercial ones. The rheology analyses showed that the amount of nanoparticles incorporated in the formulations influences the gel-like or liquid-like behavior. The results showed that the surface modified TiO2nanoparticles are a promising innovative UV filter and the formulations containing these nanoparticles are interesting candidates for being used as sunscreen.

Mesoporous Ordered Organosilicas Containing Zr and Ti Species

2010 ◽  
Vol 163 ◽  
pp. 55-58
Author(s):  
M. Zienkiewicz ◽  
Stanislaw Pikus ◽  
E. Olszewska ◽  
M. Barczak
Keyword(s):  
Photoelectron Spectroscopy ◽  
High Surface ◽  
Sol Gel ◽  
Titanium Isopropoxide ◽  
Inorganic Materials ◽  
Isomorphous Substitution ◽  
Periodic Mesoporous Organosilica ◽  
Structure Directing Agent ◽  
Surface Areas ◽  
Bridging Groups

Periodic mesoporous organosilica materials (PMOs) are the new class of porous and hybrid organic-inorganic materials. They represent exceptional and functional bridged polysilsesquioxanes prepared by sol-gel processing of monomers using triblock copolymers or ionic surfactants as the structure directing agents. By changing the monomer type, various organic functional groups may be incorporated into the framework of PMO materials. Moreover it is possible to introduce heteroatoms in the structure of mesoporous materials via isomorphous substitution of the silicon atoms. In the present study, we report the preparation and characterization of the series of zirconium, titanium and mixture of them, doped mesoporous silica. The PMOs have been synthesized by the hydrolysis and the condensation of bridged silsesquioxane precursors containing two different organic bridging groups ((R’)3Si-CH2-CH2-Si(R’)3, R’ - methoxy or ethoxy). The influence of temperature of synthesis on the structure of PMOs was examined. PMO-Zr and PMO-Zr-Ti were synthesized by employing a zirconyl chloride octahydrate (ZrOCl2•8H2O), titanium isopropoxide, NaCl, bis(trimethoxysilyl)ethane (BTME) as a silica source and triblock copolymer P123 as the structure directing agent while PMO-Ti was prepared using 1,2-bis(triethoxysilyl)ethane (BTESE), titanium isopropoxide, NaOH and cetyltrimethylammonium bromide (CTABr) as a structure directing agent. The resulting materials exhibited well-ordered two-dimensional hexagonal space group p6mm, high surface areas in the range of 700-1100 m2/g. The X-ray photoelectron spectroscopy (XPS) analysis indicated the successful incorporation of heteroatoms into hybrid PMOs and the IR spectra confirmed satisfactory removal of the surfactants.

scholarly journals “Traditional” Sol-Gel Chemistry as a Powerful Tool for the Preparation of Supported Metal and Metal Oxide Catalysts

Materials ◽  
2019 ◽  
Vol 12 (4) ◽  
pp. 668 ◽  
Author(s):  
Serena Esposito
Keyword(s):  
Metal Oxide ◽  
High Surface ◽  
Sol Gel ◽  
Chemical Properties ◽  
Inorganic Materials ◽  
Synthetic Approach ◽  
Preparation Methods ◽  
Synthesis Conditions ◽  
Molecular Precursors ◽  
Gel Preparation

The sol-gel method is an attractive synthetic approach in the design of advanced catalytic formulations that are based on metal and metal oxide with high degree of structural and compositional homogeneity. Nowadays, though it originated with the hydrolysis and condensation of metal alkoxides, sol-gel chemistry gathers plenty of fascinating strategies to prepare materials from solution state precursors. Low temperature chemistry, reproducibility, and high surface to volume ratios of obtained products are features that add merit to this technology. The development of different and fascinating procedure was fostered by the availability of new molecular precursors, chelating agents and templates, with the great advantage of tailoring the physico-chemical properties of the materials through the manipulation of the synthesis conditions. The aim of this review is to present an overview of the “traditional” sol-gel synthesis of tailored and multifunctional inorganic materials and their application in the main domain of heterogeneous catalysis. One of the main achievements is to stress the versatility of sol-gel preparation by highlighting its advantage over other preparation methods through some specific examples of the synthesis of catalysts.

COLLAPSE OF POROSITY DURING DRYING OF ALKYLENE-BRIDGED POLYSILSESQUIOXANE GELS. INFLUENCE OF THE BRIDGING GROUP LENGTH

2004 ◽  
Vol 847 ◽  
Author(s):  
Douglas A. Loy ◽  
James H. Small ◽  
Kimberly A. DeFriend ◽  
Kennard V. Wilson ◽  
McKenzie Minke ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Solid State ◽  
Solid State Nmr ◽  
Sol Gel ◽  
Network Polymer ◽  
Porous Coatings ◽  
Acidic Conditions ◽  
Bridged Polysilsesquioxane ◽  
Hybrid Xerogels ◽  
Bridging Groups

ABSTRACTThe introduction of organic substituents into sol-gel materials can often result in networks that collapse during drying to afford non-porous xerogels. This can prove useful if non-porous coatings or membranes are the ultimate objectives. Collapse of porosity is also manifested in bridged polysilsesquioxanes with flexible bridging groups. Alkylene-bridged polysilsesquioxanes are hybrid xerogels whose organic bridging group is an integral constituent of the network polymer that can be systematically varied to probe the influence of its length on the xerogels' porosity and morphology. Our previous studies have shown that hexylene-bridged polysilsesquioxane xerogels prepared from 1, 6-bis(triethoxysilyl)hexane under acidic conditions are nonporous while the pentylene-bridged polysilsesquioxanes prepared under the same conditions are porous. We also discovered that the more reactive 1, 6-bis(trimethoxysilyl)hexane monomer could polymerize under acidic conditions to afford porous xerogels. Here, we have extended our study of bis(trimethoxysilyl)alkanes to include the heptylene (C7), octylene (C8), nonylene(C9) and decylene (C10) bridges so as to ascertain at what bridging group length the porosity collapses. The morphology of the resulting xerogels was characterized by nitrogen sorption porosimetry and electron microscopy. Solid state NMR was used to structurally characterize the materials.

Cu Doped TiO2: Visible Light Assisted Photocatalytic Antimicrobial Activity and High Temperature Anatase Stability

2018 ◽  
Author(s):  
Snehamol Mathew ◽  
Priyanka Ganguly ◽  
Stephen Rhatigan ◽  
Vignesh Kumaravel ◽  
Ciara Byrne ◽  
...  
Keyword(s):  
Visible Light ◽  
Visible Light Irradiation ◽  
Density Functional ◽  
Anatase Phase ◽  
Sol Gel ◽  
Chemical Properties ◽  
Light Irradiation ◽  
Health Concern ◽  
Bacterial Inactivation ◽  
X Ray

Indoor surface contamination by microbes is a major public health concern. A damp environment is one potential sources for microbe proliferation. Smart photocatalytic coatings on building surfaces using semiconductors like titania (TiO<sub>2</sub>) can effectively curb this growing threat.<b> </b>Metal-doped titania in anatase phase has been proved as a promising candidate for energy and environmental applications. In this present work, the antimicrobial efficacy of copper (Cu) doped TiO<sub>2 </sub>(Cu-TiO<sub>2</sub>) was evaluated against <i>Escherichia coli</i> (Gram-negative) and <i>Staphylococcus aureus</i> (Gram-positive) under visible light irradiation. Doping of a minute fraction of Cu (0.5 mol %) in TiO<sub>2 </sub>was carried out <i>via</i> sol-gel technique. Cu-TiO<sub>2</sub> further calcined at various temperatures (in the range of 500 °C – 700 °C) to evaluate the thermal stability of TiO<sub>2</sub> anatase phase. The physico-chemical properties of the samples were characterised through X-ray diffraction (XRD), Raman spectroscopy, X-ray photo-electron spectroscopy (XPS) and UV-visible spectroscopy techniques. XRD results revealed that the anatase phase of TiO<sub>2</sub> was maintained well, up to 650 °C, by the Cu dopant. UV-DRS results suggested that the visible light absorption property of Cu-TiO<sub>2 </sub>was enhanced and the band gap is reduced to 2.8 eV. Density functional theory (DFT) studies emphasises the introduction of Cu<sup>+</sup> and Cu<sup>2+</sup> ions by replacing Ti<sup>4+</sup> ions in the TiO<sub>2</sub> lattice, creating oxygen vacancies. These further promoted the photocatalytic efficiency. A significantly high bacterial inactivation (99.9%) was attained in 30 mins of visible light irradiation by Cu-TiO<sub>2</sub>.

scholarly journals Physico-Chemical Investigation of Endodontic Sealers Exposed to Simulated Intracanal Heat Application: Hydraulic Calcium Silicate-Based Sealers

Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 728
Author(s):  
David Donnermeyer ◽  
Magdalena Ibing ◽  
Sebastian Bürklein ◽  
Iris Weber ◽  
Maximilian P. Reitze ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Thermal Treatment ◽  
Film Thickness ◽  
Physical Properties ◽  
Calcium Silicate ◽  
Setting Time ◽  
Chemical Properties ◽  
Chemical Changes ◽  
Time Flow ◽  
Heat Application

The aim of this study was to gain information about the effect of thermal treatment of calcium silicate-based sealers. BioRoot RCS (BR), Total Fill BC Sealer (TFBC), and Total Fill BC Sealer HiFlow (TFHF) were exposed to thermal treatment at 37 °C, 47 °C, 57 °C, 67 °C, 77 °C, 87 °C and 97 °C for 30 s. Heat treatment at 97 °C was performed for 60 and 180 s to simulate inappropriate application of warm obturation techniques. Thereafter, specimens were cooled to 37 °C and physical properties (setting time/flow/film thickness according to ISO 6876) were evaluated. Chemical properties (Fourier-transform infrared spectroscopy) were assessed after incubation of the specimens in an incubator at 37 °C and 100% humidity for 8 weeks. Statistical analysis of physical properties was performed using the Kruskal-Wallis-Test (P = 0.05). The setting time, flow, and film thickness of TFBC and TFHF were not relevantly influenced by thermal treatment. Setting time of BR decreased slightly when temperature of heat application increased from 37 °C to 77 °C (P < 0.05). Further heat treatment of BR above 77 °C led to an immediate setting. FT-IR spectroscopy did not reveal any chemical changes for either sealers. Thermal treatment did not lead to any substantial chemical changes at all temperature levels, while physical properties of BR were compromised by heating. TFBC and TFHF can be considered suitable for warm obturation techniques.

scholarly journals Technosols Development in an Abandoned Mining Area and Environmental Risk Assessment

2021 ◽  
Vol 11 (15) ◽  
pp. 6982
Author(s):  
Chiara Ferronato ◽  
Gilmo Vianello ◽  
Mauro De Feudis ◽  
Livia Vittori Antisari
Keyword(s):  
Central Italy ◽  
Organic Matter Content ◽  
Chemical Properties ◽  
Soil Surface ◽  
Mining Area ◽  
Physicochemical Characteristics ◽  
Matter Content ◽  
Mine Tailing ◽  
Inorganic Materials ◽  
Soil Features

The study of Technosols development, spatial distribution and physicochemical characteristics is becoming more and more important in the Anthropocene Era. The aim of the present study was to assess soil features and potential heavy metal release risk of soils developed on different mine tailing types after the waste disposal derived from mining activity in Central Italy. Soils were analyzed for their morphological, physical and chemical properties, and a chemical sequential extraction of heavy metals was performed. The investigated soils were classified as Technosols toxic having in some layer within 50 cm of the soil surface inorganic materials with high concentrations of toxic elements. Our findings showed that the bioavailability of potentially toxic element concentrations in the soil changed according to the origin of the mine tailing. However, because of the acidic pH, there is a serious risk of metals leaching which was reduced where the soil organic matter content was higher.

scholarly journals Green Synthesis of N/Zr Co-Doped TiO2 for Photocatalytic Degradation of p-Nitrophenol in Wastewater

Catalysts ◽  
2021 ◽  
Vol 11 (2) ◽  
pp. 235
Author(s):  
Hayette Benkhennouche-Bouchene ◽  
Julien G. Mahy ◽  
Cédric Wolfs ◽  
Bénédicte Vertruyen ◽  
Dirk Poelman ◽  
...  
Keyword(s):  
Visible Light ◽  
Tio2 Nanoparticles ◽  
Sol Gel ◽  
Visible Region ◽  
Chemical Properties ◽  
Pure Tio2 ◽  
Molar Ratio ◽  
Xps Spectra ◽  
Doped Tio2 ◽  
Co Doped

TiO2 prepared by a green aqueous sol–gel peptization process is co-doped with nitrogen and zirconium to improve and extend its photoactivity to the visible region. Two nitrogen precursors are used: urea and triethylamine; zirconium (IV) tert-butoxide is added as a source of zirconia. The N/Ti molar ratio is fixed regardless of the chosen nitrogen precursor while the quantity of zirconia is set to 0.7, 1.4, 2, or 2.8 mol%. The performance and physico-chemical properties of these materials are compared with the commercial Evonik P25 photocatalyst. For all doped and co-doped samples, TiO2 nanoparticles of 4 to 8 nm of size are formed of anatase-brookite phases, with a specific surface area between 125 and 280 m2 g−1 vs. 50 m2 g−1 for the commercial P25 photocatalyst. X-ray photoelectron (XPS) measurements show that nitrogen is incorporated into the TiO2 materials through Ti-O-N bonds allowing light absorption in the visible region. The XPS spectra of the Zr-(co)doped powders show the presence of TiO2-ZrO2 mixed oxide materials. Under visible light, the best co-doped sample gives a degradation of p-nitrophenol (PNP) equal to 70% instead of 25% with pure TiO2 and 10% with P25 under the same conditions. Similarly, the photocatalytic activity improved under UV/visible reaching 95% with the best sample compared to 50% with pure TiO2. This study suggests that N/Zr co-doped TiO2 nanoparticles can be produced in a safe and energy-efficient way while being markedly more active than state-of-the-art photocatalytic materials under visible light.

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