scholarly journals Facile Sol-gel Synthesis of Porous Silicas Using Poly(propylene)imine Dendrimers as Templates

2000 ◽  
Vol 15 (8) ◽  
pp. 1842-1848 ◽  
Author(s):  
Gustavo Larsen ◽  
Edgar Lotero ◽  
Manuel Marquez
Keyword(s):  
Single Molecule ◽  
Sol Gel ◽  
Three Dimensional ◽  
X Ray Diffraction ◽  
Template Removal ◽  
Synthesis Conditions ◽  
Transmission Electron ◽  
Argon Adsorption ◽  
Poly Propylene ◽  
Sol Gel Synthesis

Commercially available poly(propylene)imine (DAB-Am-32 and DAB-Am-64) dendrimers were used as single-molecule templates to tailor the porosity of silicas via a nonacidic sol-gel method. X-ray diffraction on both the as-prepared (oven-dried at 373 K) and the calcined (833 K) materials revealed that modest contraction took place on template removal and that the cavities created did not achieve three-dimensional ordering under the current synthesis conditions. Transmission electron microscopy of “Pt-stained” samples supported this picture. A modified Horvath–Kawazoe analysis of the argon adsorption isotherms indicated that DAB-Am-64 is a much more effective template than DAB-Am-32. Pyrolysis and oxidation protocols for template removal are also presented.

scholarly journals V2O3/C composite fabricated by carboxylic acid-assisted sol–gel synthesis as anode material for lithium-ion batteries

2021 ◽  
Author(s):  
G. S. Zakharova ◽  
E. Thauer ◽  
A. N. Enyashin ◽  
L. F. Deeg ◽  
Q. Zhu ◽  
...  
Keyword(s):  
Electrochemical Performance ◽  
Lithium Ion Batteries ◽  
Sol Gel ◽  
Carbon Sources ◽  
Lithium Ion ◽  
X Ray Diffraction ◽  
Electron Microscopies ◽  
Transmission Electron ◽  
Battery Electrode ◽  
Sol Gel Synthesis

AbstractThe potential battery electrode material V2O3/C has been prepared using a sol–gel thermolysis technique, employing vanadyl hydroxide as precursor and different organic acids as both chelating agents and carbon sources. Composition and morphology of resultant materials were characterized by X-ray diffraction, Raman spectroscopy, scanning and transmission electron microscopies, physical sorption, and elemental analysis. Stability and electronic properties of model composites with chemically and physically integrated carbon were studied by means of quantum-chemical calculations. All fabricated composites are hierarchically structured and consist of carbon-covered microparticles assembled of polyhedral V2O3 nanograins with intrusions of amorphous carbon at the grain boundaries. Such V2O3/C phase separation is thermodynamically favored while formation of vanadium (oxy)carbides or heavily doped V2O3 is highly unlikely. When used as anode for lithium-ion batteries, the nanocomposite V2O3/C fabricated with citric acid exhibits superior electrochemical performance with an excellent cycle stability and a specific charge capacity of 335 mAh g−1 in cycle 95 at 100 mA g−1. We also find that the used carbon source has only minor effects on the materials’ electrochemical performance.

Structural Characterization and CO Oxidation Activity of Nanostructured LaMnO3 Catalysts

2002 ◽  
Vol 55 (12) ◽  
pp. 757 ◽  
Author(s):  
Min Chen ◽  
Huai-Qing Huang ◽  
Xiao-Ming Zheng ◽  
Michael A. Morris
Keyword(s):  
Co Oxidation ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
Total Oxidation ◽  
Oxidation Activity ◽  
Preparation Methods ◽  
Synthesis Conditions ◽  
Nanostructured Particles ◽  
Transmission Electron ◽  
Perovskite Type

Perovskite-type LaMnO3 catalysts were prepared by three different methods and tested for CO oxidation. The structural character of the catalysts was investigated by using powder X-ray diffraction (XRD) and transmission electron microscopy (TEM). All three different preparation methods resulted in nanostructured particles forming in the LaMnO3 catalysts. The crystallite size was in the range of 20 to 80 nm depending on the synthesis conditions. It was possible to synthesize the smallest particle size and a pure phase of perovskite-type LaMnO3 oxide by using a sol–gel method. The results also indicated that the CO total oxidation activity was related to the size of LaMnO3 particle and the structure formed.

Sol-Gel Synthesis and Characterization of Nanocrystalline Bi4Ti3O12 Powders

2014 ◽  
Vol 997 ◽  
pp. 359-362 ◽  
Author(s):  
Chun Hong Ma ◽  
Xue Lin ◽  
Liang Wang ◽  
Yong Sheng Yan
Keyword(s):  
Phase Inversion ◽  
Bismuth Titanate ◽  
Sol Gel ◽  
Tetrabutyl Titanate ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Sol Gel Synthesis ◽  
Source Materials

Nanocrystalline bismuth titanate (Bi4Ti3O12; BTO) powders were successfully prepared by the sol-gel method, using bismuth nitrate (Bi(NO3)3·5H2O) and tetrabutyl titanate (Ti(OC4H9)4) as source materials, acetic anhydride and ethanediol as solvents. The thermal decomposition and phase inversion process of the gel precursors were studied by using differential thermal analysis (DTA). The crystal structures and microstructures of BTO powders were investigated by using x-ray diffraction (XRD), and transmission electron microscope (TEM). The crystallization of amorphous bismuth titanate has been discussed. The effect of sintering temperature on the structure and morphology of BTO was investigated. At 644 oC and above, BTO powder undergoes a phase transformation from tetragonal to orthorhombic. At 900 oC, the purified orthorhombic BTO nanocrystals were obtained.

Homogeneity in the Polyether Alkoxide Sol‐Gel Synthesis of YBa2Cu3O7-δ

1994 ◽  
Vol 346 ◽  
Author(s):  
Carol S. Houk ◽  
Gary A. Burgoine ◽  
Catherine J. Page
Keyword(s):  
Sol Gel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Diffraction Patterns ◽  
Mapping Techniques ◽  
Starting Solutions ◽  
Average Size ◽  
Sol Gel Synthesis ◽  
Elemental Maps

ABSTRACTWe have investigated the homogeneity of sol‐gel derived YBa2Cu307‐s from the solution phase to the final product using transmission electron microscopy (TEM), x‐ray diffraction (XRD), and Energy Dispersive X‐ray (EDX) lateral mapping techniques. The starting solutions contain stoichiometric amounts of the metal 2‐(2‐methoxyethoxy)ethoxide components in 2‐(2‐methoxyethoxy)ethanol and appear to be homogeneous by TEM with a uniform distribution of particles having an average size of less than 40 â. Through elemental mapping we see elemental segregation in the high temperature (950 °C) products, which are orthorhombic by XRD. In elemental maps of gel samples fired to 700 °C, which are tetragonal by XRD, we also see elemental inhomogeneity within particles and phase zoning in maps of products from finely ground gels. A comparison of elemental maps and x‐ray diffraction patterns of the products from gel processing and conventional solid state processing is made.

Sol–gel synthesis, structural and electrical properties of Li2CoSiO4 cathode material

2014 ◽  
Vol 07 (06) ◽  
pp. 1440001 ◽  
Author(s):  
Michał Świętosławski ◽  
Marcin Molenda ◽  
Piotr Natkański ◽  
Piotr Kuśtrowski ◽  
Roman Dziembaj ◽  
...  
Keyword(s):  
Electrical Conductivity ◽  
Sol Gel ◽  
Lithium Ion ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Structural And Electrical Properties ◽  
Potential Alternative ◽  
Sol Gel Synthesis ◽  
First Time

Polyanionic cathode materials for lithium-ion batteries start to be considered as potential alternative for layered oxide materials. Among them, Li 2 CoSiO 4, characterized by outstanding capacity and working voltage, seems to be an interesting substitute for LiFePO 4 and related systems. In this work, structural and electrical investigations of Li 2 CoSiO 4 obtained by sol–gel synthesis were presented. Thermal decomposition of gel precursor was studied using EGA (FTIR)-TGA method. Chemical composition of the obtained material was confirmed using X-ray diffraction and energy-dispersive X-ray spectroscopy. The morphology of β- Li 2 CoSiO 4 was studied using transmission electron microscopy. High temperature electrical conductivity of Li 2 CoSiO 4 was measured for the first time. Activation energies of the electrical conductivity of two Li 2 CoSiO 4 polymorphs (β and γ) were determined. The room temperature electrical conductivity of those materials was estimated as well.

scholarly journals Sol-Gel Derived Eu3+-Doped Gd2Ti2O7Pyrochlore Nanopowders

2015 ◽  
Vol 2015 ◽  
pp. 1-8 ◽  
Author(s):  
Sanja Ćulubrk ◽  
Željka Antić ◽  
Vesna Lojpur ◽  
Milena Marinović-Cincović ◽  
Miroslav D. Dramićanin
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Structural Changes ◽  
Sol Gel ◽  
Pyrochlore Phase ◽  
Structural Defects ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Sol Gel Synthesis

Herein we presented hydrolytic sol-gel synthesis and photoluminescent properties of Eu3+-doped Gd2Ti2O7pyrochlore nanopowders. According to Gd2Ti2O7precursor gel thermal analysis a temperature of 840°C is identified for the formation of the crystalline pyrochlore phase. Obtained samples were systematically characterized by powder X-ray diffraction, scanning and transmission electron microscopy, and photoluminescence spectroscopy. The powders consist of well-crystalline cubic nanocrystallites of approximately 20 nm in size as evidenced from X-ray diffraction. The scanning and transmission electron microscopy shows that investigated Eu3+-doped Gd2Ti2O7nanopowders consist of compact, dense aggregates composed entirely of nanoparticles with variable both shape and dimension. The influence of Eu3+ions concentration on the optical properties, namely, photoluminescence emission and decay time, is measured and discussed. Emission intensity as a function of Eu3+ions concentration shows that Gd2Ti2O7host can accept Eu3+ions in concentrations up to 10 at.%. On the other hand, lifetime values are similar up to 3 at.% (~2.7 ms) and experience decrease at higher concentrations (2.4 ms for 10 at.% Eu3+). Moreover, photoluminescent spectra and lifetime values clearly revealed presence of structural defects in sol-gel derived materials proposing photoluminescent spectroscopy as a sensitive tool for monitoring structural changes in both steady state and lifetime domains.

Sol-gel synthesis of silica–based mesoporous powders

2004 ◽  
Vol 848 ◽  
Author(s):  
Lidia Armelao ◽  
Gregorio Bottaro ◽  
Renzo Campostrini ◽  
Stefano Gialanella ◽  
Marco Ischia ◽  
...  
Keyword(s):  
Sol Gel ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
Structure Directing Agent ◽  
Template Removal ◽  
Guest Species ◽  
Poly Ethylene Oxide ◽  
Acidic Conditions ◽  
Poly Ethylene ◽  
Sol Gel Synthesis

ABSTRACTMesoporous silica powders have been synthesized starting from aqueous solutions of Si(OCH2CH3)4 (TEOS) under acidic conditions, using non-ionic alkyl poly(ethylene oxide) oligomer (Brij76) as a structure-directing agent. Template removal was performed by thermal treatment in air as well as by ethanol extraction. The annealing process (400 - 600°C) resulted in more efficient elimination of the organic molecules, thus yielding hexagonal (p6mm) mesopor-ous materials with pore volume and specific surface area ranging between 0.58 – 0.41 cm3/g and 900 – 700 m2/g, respectively. The systems were characterized by X-Ray Diffraction (XRD), N2 BET adsorption, Thermogravimetric Analysis (TGA) and Differential Scanning Calorimetry (DSC). Particular attention was focused on the evolution of the system mesostructural and porous features as a function of the template removal procedure. The obtained mesoporous networks are suitable as matrices for the development of nanocomposite systems in which the dispersion or the growth of various guest species (clusters, molecules…) can be addressed into the host mesopores.

scholarly journals Novel Sol-Gel Synthesis of Spherical Lead Titanate Submicrometer Powders

Crystals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 484
Author(s):  
Radhouane Bel-Hadj-Tahar ◽  
Mohamed Abboud ◽  
Mohd. Shkir ◽  
Abdullah Alhanash ◽  
Ali Eisa M. Anqi ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Lead Titanate ◽  
Sol Gel ◽  
Particle Morphology ◽  
Submicron Particles ◽  
X Ray Diffraction ◽  
Synthetic Process ◽  
Transmission Electron ◽  
Autogenous Pressure ◽  
Sol Gel Synthesis

In this study, a novel and simple synthetic sol-gel procedure was established to directly prepare spherical lead titanate powders without prior synthesis/usage of spherical templates such as TiO2 particles. Isotropic submicron particles with a mean diameter of 1–4 μm were prepared in this way. This synthetic process takes advantage of acetone as a stabilizing ligand and autogenous pressure generated in the autoclave during the reaction. The influence of various experimental factors (nature of the ligand, thermal treatment mode, and post-calcining temperature) as well as the formation mechanism were studied. Scanning electron microscopy and transmission electron microscopy were used to explore the particle morphology. The crystalline phases were explored and identified by X-ray diffraction analysis.

Pure and Ca-doped LaCoO3 Nanopowders: Sol-Gel Synthesis, Characterization and Magnetic Properties

2004 ◽  
Vol 848 ◽  
Author(s):  
Lidia Armelao ◽  
Davide Barreca ◽  
Gregorio Bottaro ◽  
Andrea Caneschi ◽  
Claudio Sangregorio ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Transmission Electron Microscopy ◽  
Magnetic Properties ◽  
Chemical Composition ◽  
Auger Electron ◽  
Sol Gel ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Sol Gel Synthesis

ABSTRACTThis work is focused on the sol-gel synthesis of pure and Ca-doped LaCoO3 nanopowders. The samples were prepared starting from methanolic solutions of cobalt (II) acetate (Co(CH3COO)2·4H2O), lanthanum (III) nitrate (La(NO3)3·6H2O) and calcium (II) acetate (Ca(CH3COO)2·H2O). After solvent evaporation, the obtained powders were dried under vacuum and subsequently treated in air up to 1273 K. The system evolution under thermal annealing was studied by X-ray Diffraction (XRD) and Transmission Electron Microscopy (TEM), while the chemical composition was analyzed by X-ray Photoelectron (XPS) and X-ray Excited Auger electron (XE-AES) spectroscopies. The temperature and field dependence of the magnetic properties of the Ca-doped samples were investigated, and compared to those of the corresponding pure LaCoO3 powders.

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