Sol-Gel Synthesis and Characterization of Barium Lanthanum Titanate Ceramics

2012 ◽  
Vol 730-732 ◽  
pp. 141-146 ◽  
Author(s):  
Katarzyna Osinska ◽  
Grzegorz Smalarz ◽  
Beata Wodecka-Dus ◽  
Dionizy Czekaj

The (Ba1-xLax)Ti1-x/4O3 (BLT) ceramics for lanthanum content x in the range 0£x£0.005 were prepared by the sol-gel method. Barium acetate, lanthanum acetate and titanium (IV) propoxide were used as starting materials. Glacial acetic acid and n-propyl alcohol were used as solvents and acetyloacetone was added as stabilizer, followed by hydrolysis. Thermal evolution of the dried gel as well as ceramic powder was studied by simultaneous thermal analysis. The amorphous gel of BLT was calcined in the furnace and pressed into pellets. The compacts were next sintered at temperature T=1100°C. The crystalline structure of BLT ceramics was studied by X-ray diffraction method. Morphology of BLT ceramics was studied by scanning electron microscopy.

2013 ◽  
Vol 58 (4) ◽  
pp. 1305-1308 ◽  
Author(s):  
B. Wodecka-Duś ◽  
M. Plońska ◽  
D. Czekaj

Abstract In the present study BaTiO3 and Ba1-xLaxTiO3 (0.1-0.4mol.% La) ceramic powders were synthesized by the conventional mixed oxide method (MOM). The characterization of the ceramic powders was carried out using a simultaneous thermal analysis (STA), with a combined DTA/TG/DTG system (Netzsch STA409). The results of thermal analysis allowed to determine the optimal temperature of synthesis. Microstructure was investigated by scanning electron microscopy (SEM), crystalline structure was studied by X-ray diffraction method (XRD). The EDS investigations showed that samples exhibited conservation of stoichiometry according to the chemical composition formula. The X-ray diffraction analysis confirmed formation of the desired crystalline structure both pure and La3+-doped BaTiO3 ceramics exhibiting a perovskite-type structure ABO3 with tetragonal symmetry P4 mm.


Materials ◽  
2021 ◽  
Vol 14 (4) ◽  
pp. 854
Author(s):  
Antonia Hoppe ◽  
Cornelius Dirksen ◽  
Karl Skadell ◽  
Michael Stelter ◽  
Matthias Schulz ◽  
...  

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.


Author(s):  
G. S. Zakharova ◽  
E. Thauer ◽  
A. N. Enyashin ◽  
L. F. Deeg ◽  
Q. Zhu ◽  
...  

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.


2009 ◽  
Vol 24 (8) ◽  
pp. 2541-2546 ◽  
Author(s):  
Eisuke Yokoyama ◽  
Hironobu Sakata ◽  
Moriaki Wakaki

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.


2013 ◽  
Vol 2013 ◽  
pp. 1-7 ◽  
Author(s):  
Thilagavathi Thirugnanam

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.


2012 ◽  
Vol 730-732 ◽  
pp. 100-104
Author(s):  
Agata Lisińska-Czekaj

In the present study Bi6Fe2Ti3O18 (BFTO) ceramics has been fabricated by solid state reaction from the mixture of simple oxides viz. Bi2O3, TiO2 and Fe2O3. Stoichiometric mixture of the powders was thermally analyzed so parameters of the thermal treatment were determined. The EDS measurements have shown conservation of the chemical composition of the ceramic powder after calcination. Hot-pressing method was used for final densification of ceramic samples. The crystalline structure of the sintered samples was examined by X-ray diffraction method at room temperature. It was found that BFTO ceramics sintered at T=980 °C adopted the orthorhombic structure of Aba2 (41) space group with the following elementary cell parameters: a=5.4567(2)Å, b=49.418(2) and c=5.4826(2). Details concerning the atom’s positions are presented.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Ekaterina V. Borisova ◽  
Alexey V. Ignatov ◽  
Eugeni I. Get'man ◽  
Stanislav N. Loboda ◽  
Lyudmyla I. Ardanova ◽  
...  

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.


2018 ◽  
Vol 762 ◽  
pp. 273-277
Author(s):  
Anzelms Zukuls ◽  
Gundars Mežinskis ◽  
Aigars Reinis ◽  
Ingus Skadins ◽  
Juta Kroica ◽  
...  

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.


2014 ◽  
Vol 997 ◽  
pp. 359-362 ◽  
Author(s):  
Chun Hong Ma ◽  
Xue Lin ◽  
Liang Wang ◽  
Yong Sheng Yan

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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