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 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.

Preparation of Nanosized TiO2 Synthesized by Sol-Gel Pathway Using Ionic Liquid as Assistant and its Photocatalytic Activities

2012 ◽  
Vol 535-537 ◽  
pp. 2240-2244
Author(s):  
Wei Wei ◽  
Chang Shun Yu ◽  
Shao Jun Wang ◽  
Qing Da An
Keyword(s):  
Ionic Liquid ◽  
Diffuse Reflectance ◽  
Sol Gel ◽  
Rutile Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Photocatalytic Activities ◽  
Average Size ◽  
Nanosized Tio2

Nanosized TiO2 particles were synthesized by sol-gel method using ionic liquid as assistant. The samples were characterized by UV-vis diffuse reflectance spectra, X-ray diffraction (XRD), transmission electron microscopy (TEM). It was shown that the phase detectable was mainly rutile phase with uniform sphericity and the average size was 10nm. Along with the rise of sintering temperature, grain diameter became bigger. The photocatalytic activities of nanosized TiO2 were evaluated by the reduction yield in the presence of CO2 and water. The result showed that TiO2 catalysts has efficient photocatalytic activities, of which made with [OMIM]BF4 displayed the highest photocatalytic active in the experiment.

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.

Sol-Gel Synthesis of the Strontium-Copper Oxycarbonate Superconductor Sr2CuO2(CO3)1−x(BO3)x

1996 ◽  
Vol 453 ◽  
Author(s):  
Audrey J. Babcock ◽  
Alexander R. Pico ◽  
Catherine J. Page
Keyword(s):  
Ambient Pressure ◽  
Sol Gel ◽  
Subsequent Treatment ◽  
Nominal Composition ◽  
Gravimetric Analysis ◽  
X Ray Diffraction ◽  
X Ray ◽  
Gel Preparation ◽  
Starting Solutions ◽  
Sol Gel Synthesis

AbstractWe have developed an ambient-pressure sol-gel synthetic route to superconducting borate-doped Sr2CuO2(CO3) using polyether alkoxide precursors. In our sol-gel preparation, the starting solutions contain strontium and copper alkoxide complexes in 2-(2-methoxy-ethoxy)ethanol. Boron is incorporated into the solution by using an aqueous boric acid solution for hydrolysis. Dried gels were examined by x-ray diffraction and thermal gravimetric analysis. By experimenting with various firing sequences and atmospheres we have established a successful route for reproducibly preparing relatively pure Sr2CuO2CO3 and boron-doped phases. Final products were characterized by x-ray diffraction, elemental analysis and magnetic susceptibility. Samples of nominal composition Sr2CuO2(CO3)0.85(BO2)0.15 are superconducting with a Tc(onset) of ∼25K. Subsequent treatment at 1100°C and 3 GPa for one hour increased Tc(onset) to ∼35K.

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 Synthesized SnO2 Nanoparticles and Their Properties

2007 ◽  
Vol 7 (12) ◽  
pp. 4402-4411 ◽  
Author(s):  
Soumen Das ◽  
Soumen Basu ◽  
Gautam Majumdar ◽  
Dipankar Chakravorty ◽  
S. Chaudhuri
Keyword(s):  
Sno2 Nanoparticles ◽  
Sol Gel ◽  
Binding Energies ◽  
X Ray Diffraction ◽  
X Ray ◽  
Optical Absorbance ◽  
Atomic Force ◽  
Transmission Electron ◽  
Average Size ◽  
Theoretical Results

Sol–gel synthesized SnO2 nanoparticles with an average size of 2.0 nm obtained at 373 K were gradually annealed to 673 K in air for 25 minutes. Sequentially taken transmission electron microscopy (TEM) images showed that particle agglomeration of these non-matrix SnO2 nanocrystals was a very slow process. The blue shifts of the band gap (∼ 2.3 eV) obtained from the optical absorbance spectra were matched with the theoretical results of the size related excitonic binding energies. These calculations also supported the observed slow grain growth. The depth sensitive hardness measurements of the thin films indicated hardness in the range of 5.03 GPa to 6.79 GPa. These undoped and non-matrix SnO2 nanoparticles were also investigated with the X-ray photoelectrons spectroscopy (XPS), atomic force microscope (AFM), X-ray diffraction spectroscopy (XRD), and ac impedance analyzer.

scholarly journals Doped Nanoscale NMC333 as Cathode Materials for Li-Ion Batteries

Materials ◽  
2019 ◽  
Vol 12 (18) ◽  
pp. 2899 ◽  
Author(s):  
Hashem ◽  
Abdel-Ghany ◽  
Scheuermann ◽  
Indris ◽  
Ehrenberg ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Sol Gel ◽  
Chelating Agent ◽  
Li Ion Batteries ◽  
X Ray Diffraction ◽  
Al Doping ◽  
X Ray ◽  
Transmission Electron ◽  
Li Ion ◽  
Diffraction Patterns

A series of Li(Ni1/3Mn1/3Co1/3)1−xMxO2 (M = Al, Mg, Zn, and Fe, x = 0.06) was prepared via sol-gel method assisted by ethylene diamine tetra acetic acid as a chelating agent. A typical hexagonal α-NaFeO2 structure (R-3m space group) was observed for parent and doped samples as revealed by X-ray diffraction patterns. For all samples, hexagonally shaped nanoparticles were observed by scanning electron microscopy and transmission electron microscopy. The local structure was characterized by infrared, Raman, and Mössbauer spectroscopy and 7Li nuclear magnetic resonance (Li-NMR). Cyclic voltammetry and galvanostatic charge-discharge tests showed that Mg and Al doping improved the electrochemical performance of LiNi1/3Mn1/3Co1/3O2 in terms of specific capacities and cyclability. In addition, while Al doping increases the initial capacity, Mg doping is the best choice as it improves cyclability for reasons discussed in this work.

scholarly journals Structural, Optical, and Photocatalytic Properties of ZnSe Nanoparticles Influenced by the Milling Time

Crystals ◽  
2021 ◽  
Vol 11 (9) ◽  
pp. 1125
Author(s):  
Bui Thi Thu Hien ◽  
Vu Thanh Mai ◽  
Pham Thi Thuy ◽  
Vu Xuan Hoa ◽  
Tran Thi Kim Chi
Keyword(s):  
Raman Spectra ◽  
Milling Time ◽  
Blue Emission ◽  
Near Band Edge ◽  
X Ray Diffraction ◽  
Znse Nanoparticles ◽  
X Ray ◽  
Transmission Electron ◽  
Diffraction Patterns ◽  
Average Size

ZnSe nanoparticles (NPs) were prepared by combining both hydrothermal and mechanical milling methods. Transmission electron microscopy images show that fabricated ZnSe NPs with a sphere-like shape have an average size (d) in the range of 20–100 nm, affected by changing the milling time from 10 to 60 min. All the samples crystalize in zincblende-type structure without impurities, as confirmed by analyzing X-ray diffraction patterns, Raman spectra, and energy-dispersive X-ray spectroscopy. Carefully checking Raman spectra, we have observed the broadening and redshift of vibration modes as decreasing NP size, which are ascribed to extra appearance of disorder and defects. The photoluminescence study has found a blue emission at 462 nm attributed to the excitonic near-band edge and a broad defect-related emission around 520–555 nm. Increasing milling time leads to the decrease in the exciton-emission intensity, while the defect-related emissions increase gradually. Interestingly, as decreasing d, we have observed an improved photodegradation of Rhodamine B under UV irradiation, proving application potentials of ZnSe NPs in photocatalytic activity.

Synthesis and Characterization of CoMn2O4 Nanopowders by a Reverse Micelle Processing

2016 ◽  
Vol 868 ◽  
pp. 105-110
Author(s):  
Dong Sik Bae
Keyword(s):  
Reverse Micelle ◽  
Molar Ratio ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Xrd Diffraction ◽  
Transmission Electron ◽  
Diffraction Patterns ◽  
Average Size

CoMn2O4 nanoparticles were synthesized by reverse micelle processing from the mixed precursor (consisting of Co (NO3)2 ·6H2O and MnCl2·4H2O). The CoMn2O4 was prepared by mixing the aqueous solution at a molar ratio of Co : Mn = 1 : 2. The synthesized powders were calcined at 600°C for 2h. The average size and distribution of synthesized powders were in the range of 10-20nm and narrow, respectively. The average size of the synthesized powders increased with increasing water to surfactant molar ratio. The XRD diffraction patterns show that the phase of CoMn2O4 was spinel (JCPDS no.77-0471). The synthesized and calcined powders were characterized by thermogravimetry-differential scanning calorimeter (TG-DSC), X-ray diffraction analysis (XRD) and transmission electron microscopy (TEM). The magnetic property of the powder was measured by Vibrating Sample Magneto-meter (VSM) at 298K. The effect of synthesis parameter, such as the molar ratio of water to surfactant, is discussed.

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