Formation of Nanostructured Energetic Materials via Modified Sol-Gel Synthesis

2003 ◽  
Vol 800 ◽  
Author(s):  
Jeremy Walker ◽  
Rina Tannenbaum
Keyword(s):  
Succinic Acid ◽  
Propylene Oxide ◽  
Energetic Materials ◽  
Sol Gel ◽  
Interfacial Area ◽  
X Ray Diffraction ◽  
Ph Profile ◽  
Carboxylate Groups ◽  
Sol Gel Synthesis ◽  
And Control

ABSTRACTThis study is concerned with the development of a modified sol-gel synthesis of Fe2O3 xerogels that would allow the design and control of the interfacial area between the oxidant iron oxide matrix and the metal reducing agent, thus optimizing the energetic yield of these highly energetic reactions. The modification consisted in the addition of a new class of di-functional template molecules, such as diamines or di-acids, as gelation agents. pH profile measurements indicated that the mechanism of reaction of propylene oxide and of succinic acid as the gelation agents was fundamentally different. Propylene oxide acts as a proton scavenger, reducing the hydrated iron species to Fe2O3, thus reducing the concentration of protons in the reaction mixture leading to an increase in pH. When succinic acid is used as the gelation agent, a decrease in pH versus time during the reaction indicates the formation of carboxylate ions, thus creating reactive molecules that are capable of stabilizing the Fe2O3 clusters during the growth process. Infrared spectra of the products in both reactions support presence of carboxylate groups in the Fe2O3 xerogels. X-ray diffraction analyses revealed low levels of crystallinity in both products, and the presence of different phases of Fe2O3.

Facile Sol-Gel Synthesis of Mesoporous TiO2 in Ionic Liquids

2013 ◽  
Vol 389 ◽  
pp. 53-56
Author(s):  
Shu Guo ◽  
Sheng Xu Lu ◽  
Hui Ding ◽  
Zai Feng Shi
Keyword(s):  
Electron Microscopy ◽  
Room Temperature ◽  
Sol Gel ◽  
Rutile Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Carboxylate Groups ◽  
Transmission Electron ◽  
Xrd Patterns ◽  
Sol Gel Synthesis

The mesoporous TiO2 particles was conveniently prepared in a room temperature ionic liquid (RTILs) of 1, 3-di-(3-propionyloxy) imdazolium tetrafluoroborate [DiprCOOBF4 system. The obtained materials were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), and N2 adsorptiondesorption analysis. XRD patterns revealed that only rutile phase is formed in the RTILs. The TEM micrographs as well as N2 adsorptiondesorption measurements show that the prepared products exhibited wormlike pore structures. The FTIR (Fourier Transform Infrared Spectra) demonstrate the carboxylate groups attach via bidentate or bridging coordination to the TiO2 surface.

scholarly journals Sodium Solid Electrolytes: NaxAlOy Bilayer-System Based on Macroporous Bulk Material and Dense Thin-Film

Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 854
Author(s):  
Antonia Hoppe ◽  
Cornelius Dirksen ◽  
Karl Skadell ◽  
Michael Stelter ◽  
Matthias Schulz ◽  
...  
Keyword(s):  
Pore Size ◽  
Bulk Material ◽  
Sol Gel ◽  
Dense Layer ◽  
X Ray Diffraction ◽  
Bilayer System ◽  
Step Procedure ◽  
Short Circuits ◽  
Α Al2o3 ◽  
Sol Gel Synthesis

A new preparation concept of a partially porous solid-state bilayer electrolyte (BE) for high-temperature sodium-ion batteries has been developed. The porous layer provides mechanical strength and is infiltrated with liquid and highly conductive NaAlCl4 salt, while the dense layer prevents short circuits. Both layers consist, at least partially, of Na-β-alumina. The BEs are synthesized by a three-step procedure, including a sol-gel synthesis, the preparation of porous, calcined bulk material, and spin coating to deposit a dense layer. A detailed study is carried out to investigate the effect of polyethylene oxide (PEO) concentration on pore size and crystallization of the bulk material. The microstructure and crystallographic composition are verified for all steps via mercury intrusion, X-ray diffraction, and scanning electron microscopy. The porous bulk material exhibits an unprecedented open porosity for a NaxAlOy bilayer-system of ≤57% with a pore size of ≈200–300 nm and pore volume of ≤0.3 cm3∙g−1. It contains high shares of crystalline α-Al2O3 and Na-β-alumina. The BEs are characterized by impedance spectroscopy, which proved an increase of ionic conductivity with increasing porosity and increasing Na-β-alumina phase content in the bulk material. Ion conductivity of up to 0.10 S∙cm−1 at 300 °C is achieved.

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.

Sol-gel synthesis and characterization of Ag nanoparticles in ZrO2 thin films

2009 ◽  
Vol 24 (8) ◽  
pp. 2541-2546 ◽  
Author(s):  
Eisuke Yokoyama ◽  
Hironobu Sakata ◽  
Moriaki Wakaki
Keyword(s):  
Thin Films ◽  
Sol Gel ◽  
Composite Films ◽  
Dip Coating ◽  
Molar Ratio ◽  
X Ray Diffraction ◽  
Silver Surface ◽  
Molar Ratios ◽  
Sol Gel Synthesis

ZrO2 thin films containing silver nanoparticles were prepared using the sol-gel method with Ag to Zr molar ratios [Ag]/[Zr] = 0.11, 0.25, 0.43, 0.67, 1.00, 1.50, and 2.33. After dip coating on glass substrate, coated films were annealed at 200 and 300 °C in air. X-ray diffraction peaks corresponding to crystalline Ag were observed, but a specific peak corresponding to ZrO2 was not observed. At the molar ratio [Ag]/[Zr] = 0.25, the particle size of Ag distributed broadly centered at 17 nm for an annealing temperature of 200 °C and at 25 nm for 300 °C. The films annealed in air at 200 °C showed an absorption band centered at 450 nm because of the silver surface plasmon resonance, whereas films heated at 300 °C in air caused a red shift of the absorption to 500 nm. The absorption peak was analyzed using the effective dielectric function of Ag-ZrO2 composite films modeled with the Maxwell-Garnett expression.

scholarly journals Effect of Polymers (PEG and PVP) on Sol-Gel Synthesis of Microsized Zinc Oxide

2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Thilagavathi Thirugnanam
Keyword(s):  
Sol Gel ◽  
Cost Effective ◽  
X Ray Diffraction ◽  
X Ray ◽  
Structural Modifications ◽  
Phase Pure ◽  
Sol Gel Synthesis ◽  
Polyethylene Glycol 6000 ◽  
Granular Morphology ◽  
Scanning Electron

Fibers irregular and seed-like microcrystalline ZnO were synthesized by using a cost-effective and low temperature aqueous sol-gel method. Various polymers, namely, polyethylene glycol 6000 (PEG 6000) and polyvinyl pyrrolidone (PVP), were used as structure directing agents. The samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The X-ray diffraction pattern revealed the formation of phase-pure ZnO micropowders. It is observed that the polymers play an important role in modifying the surface morphology and the size of the crystallites. A compact granular morphology is observed for the ZnO samples without polymer. The samples exhibit microparticles of size 100 nm for PVP and for PEG-mediated growth, whereas microporous corrugated morphology is observed for added PEG-mediated micropowder. FTIR study is used to confirm the structural modifications occurring in the polymers.

scholarly journals Alumina-Doped Zirconia Submicro-Particles: Synthesis, Thermal Stability, and Microstructural Characterization

Materials ◽  
2019 ◽  
Vol 12 (18) ◽  
pp. 2856 ◽  
Author(s):  
Gregor Thomas Dahl ◽  
Sebastian Döring ◽  
Tobias Krekeler ◽  
Rolf Janssen ◽  
Martin Ritter ◽  
...  
Keyword(s):  
Grain Growth ◽  
Sol Gel ◽  
Microstructural Characterization ◽  
Alumina Content ◽  
Stabilizing Agents ◽  
Precise Control ◽  
Size And Shape ◽  
Elemental Analyses ◽  
Sol Gel Synthesis ◽  
And Control

Zirconia nanoceramics are interesting materials for numerous high-temperature applications. Because their beneficial properties are mainly governed by the crystal and microstructure, it is essential to understand and control these features. The use of co-stabilizing agents in the sol-gel synthesis of zirconia submicro-particles should provide an effective tool for adjusting the particles’ size and shape. Furthermore, alumina-doping is expected to enhance the particles’ size and shape persistence at high temperatures, similar to what is observed in corresponding bulk ceramics. Dispersed alumina should inhibit grain growth by forming diffusion barriers, additionally impeding the martensitic phase transformation in zirconia grains. Here, alumina-doped zirconia particles with sphere-like shape and average diameters of ∼ 300 n m were synthesized using a modified sol-gel route employing icosanoic acid and hydroxypropyl cellulose as stabilizing agents. The particles were annealed at temperatures between 800 and 1200 ∘ C and characterized by electron microscopy, elemental analysis, and X-ray diffraction. Complementary elemental analyses confirmed the precise control over the alumina content (0–50 mol%) in the final product. Annealed alumina-doped particles showed more pronounced shape persistence after annealing at 1000 ∘ C than undoped particles. Quantitative phase analyses revealed an increased stabilization of the tetragonal/cubic zirconia phase and a reduced grain growth with increasing alumina content. Elemental mapping indicated pronounced alumina segregation near the grain boundaries during annealing.

scholarly journals Sol-Gel Synthesis, X-Ray Diffraction Studies, and Electric Conductivity of Sodium Europium Silicate

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Ekaterina V. Borisova ◽  
Alexey V. Ignatov ◽  
Eugeni I. Get'man ◽  
Stanislav N. Loboda ◽  
Lyudmyla I. Ardanova ◽  
...  
Keyword(s):  
Activation Energy ◽  
Electric Conductivity ◽  
Rietveld Refinement ◽  
Sol Gel ◽  
Apatite Structure ◽  
X Ray Diffraction ◽  
Gel Method ◽  
X Ray ◽  
Sol Gel Method ◽  
Sol Gel Synthesis

Sodium europium silicate, NaEu9(SiO4)6O2, with apatite structure has been obtained and studied using X-ray diffraction and SEM. It has been shown that sodium sublimation does not take place upon synthesis by the sol-gel method. Rietveld refinement has revealed that sodium atoms are ordered and occupy the 4f position. O(4) atoms not related to silicate ions are placed at the centers of Eu(2) triangles. DC and AC electric conductivity and activation energy have been determined for the compound studied.

Sol-Gel Synthesis of SnO2-TiO2 System - Morphologic, Photocatalytic and Antibacterial Properties

2018 ◽  
Vol 762 ◽  
pp. 273-277
Author(s):  
Anzelms Zukuls ◽  
Gundars Mežinskis ◽  
Aigars Reinis ◽  
Ingus Skadins ◽  
Juta Kroica ◽  
...  
Keyword(s):  
Sol Gel ◽  
Antibacterial Properties ◽  
Soda Lime ◽  
Rutile Phase ◽  
X Ray Diffraction ◽  
Oxide Coatings ◽  
Atomic Force ◽  
Heat Treated ◽  
Soda Lime Silicate Glass ◽  
Sol Gel Synthesis

SnO2-TiO2 sol-gel coatings on soda-lime silicate glass heat treated at 500 °C and xerogel specimens also heat treated at 500 °C were investigated in this study. The morphology of 1, 3, 5 and 7 mol% SnO2 doped titanium oxide coatings were evaluated with a scanning electron microscope (SEM), an atomic force microscope (AFM) and an UV-VIS light spectrophotometer, whilst xerogel structure was analysed with X-ray diffraction spectroscopy (XRD). The physicochemical properties of the TiO2-SnO2 systems depended mainly on the Sn-to-Ti ratio. The surface morphology of the layer was compact and homogeneous with no visible cracks. Anatase and rutile phase was found in the tested 1, 3, 5, 7 and 10 mol% SnO2 doped and heat treated xerogel specimens. Rutile phase content in the heat treated xerogel was reduced, if Sn4+ content was increased. Photocatalytic activity and antibacterial properties were evaluated as well.

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.

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