Thermal and structural characterization of the ZrO2−x(OH)2xto ZrO2 transition

2001 ◽  
Vol 16 (8) ◽  
pp. 2209-2212 ◽  
Author(s):  
E Torres-GarciÁa ◽  
A. Peláiz-Barranco ◽  
C. Vázquez-Ramos ◽  
G. A. Fuentes

The exothermic process that occurs around 700 K during calcination of ZrO2−x(OH)2x, associated with the crystallization of the low-temperature tetragonal metastable phase of ZrO2, was analyzed using x-ray diffraction, high-resolution thermogravimetric analysis (TGA), nitrogen adsorption, and modulated differential scanning calorimetry (MDSC). High-resolution TGA allowed us to determine the water loss, resulting from condensation of OH− groups. The amount was 0.137 wt% in our case, equivalent to 1.7 × 10−2 mol of H2O/mol of ZrO2. That corresponds to about one −OH group per nm2 being lost in that process. By using MDSC we determined that the change in enthalpy (∆Hglobal = −15.49 kJ/mol of ZrO2) was the result of two parallel contributions. One of them was reversible and endothermic (∆Hrev = 0.11 kJ/mol of ZrO2), whereas the other was irreversible and exothermic (∆Hirrev = −15.60 kJ/mol of ZrO2). The variability and magnitude of the exotherm, as well as the fact that the accompanying weight loss is so small, are consistent with a mechanism involving the formation of tetragonal nuclei, rather than global crystallization, and hence depend on the number of nuclei so formed.

Author(s):  
D. Nagasamy Venkatesh ◽  
S. Karthick ◽  
M. Umesh ◽  
G. Vivek ◽  
R.M. Valliappan ◽  
...  

Roxythromycin/ β-cyclodextrin (Roxy/ β-CD) dispersions were prepared with a view to study the influence of β-CD on the solubility and dissolution rate of this poorly soluble drug. Phase-solubility profile indicated that the solubility of roxythromycin was significantly increased in the presence of β-cyclodextrin and was classified as AL-type, indicating the 1:1 stoichiometric inclusion complexes. Physical characterization of the prepared systems was carried out by differential scanning calorimetry (DSC), X-ray diffraction studies (XRD) and IR studies. Solid state characterization of the drug β-CD binary system using XRD, FTIR and DSC revealed distinct loss of drug crystallinity in the formulation, ostensibly accounting for enhancement of dissolution rate.


2015 ◽  
Vol 48 (2) ◽  
pp. 528-532 ◽  
Author(s):  
Peter Zaumseil

The occurrence of the basis-forbidden Si 200 and Si 222 reflections in specular X-ray diffraction ω–2Θ scans is investigated in detail as a function of the in-plane sample orientation Φ. This is done for two different diffractometer types with low and high angular divergence perpendicular to the diffraction plane. It is shown that the reflections appear for well defined conditions as a result of multiple diffraction, and not only do the obtained peaks vary in intensity but additional features like shoulders or even subpeaks may occur within a 2Θ range of about ±2.5°. This has important consequences for the detection and verification of layer peaks in the corresponding angular range.


Author(s):  
S. Louki ◽  
N. Touach ◽  
A. Benzaouak ◽  
V. M. Ortiz-Martínez ◽  
M. J. Salar-García ◽  
...  

This work investigates the photocatalytic activity of new ferroelectric material with formula (Li0.95Cu0.15)Ta0.76Nb0.19O3 (LT76) in a single chamber microbial fuel cell (MFC) and compares its performance with the similar photocatalyst (Li0.95Cu0.15)Ta0.57Nb0.38O3 (LT57). The photocatalysts LT76 and LT57 were synthesized by ceramic route under the same conditions, with the same starting materials. The ratio Ta/Nb was fixed at 4.0 and 1.5 for LT76 and LT57, respectively. These phases were characterized by different techniques including X-ray diffraction (XRD), transmission electronic microscopy (TEM), particle size distribution (PSD), differential scanning calorimetry (DSC), and ultraviolet (UV)–visible (Vis). The new photocatalyst LT76 presents specific surface area of 0.791 m2/g and Curie temperature of 1197 °C. The photocatalytic efficiency of this material is assessed in terms of wastewater treatment and electricity generation by power density and removal rate of chemical oxygen demand (COD) in the presence of a light source. The values of maximum power density and COD removal were 19.77 mW/m3 and 93%, respectively, for LT76.


1997 ◽  
pp. 439-448 ◽  
Author(s):  
A. Sanz-Hervás ◽  
C. Villar ◽  
M. Aguilar ◽  
A. Sacedón ◽  
J. L. Sánchez-Rojas ◽  
...  

Molecules ◽  
2020 ◽  
Vol 25 (23) ◽  
pp. 5552
Author(s):  
Ryota Kudo ◽  
Masahiro Sonobe ◽  
Yoshiaki Chino ◽  
Yu Kitazawa ◽  
Mutsumi Kimura

The synthesis and characterization of two phthalocyanine (Pc) structural isomers, 1 and 2, in which four 2,6-di(hexyloxy)phenyl units were attached directly to the 1,8,15,22- or 1,4,15,18-positions of the Pc rings, are described. Both Pcs 1 and 2 exhibited low melting points, i.e., 120 and 130 °C respectively, due to the reduction in intermolecular π-π interaction among the Pc rings caused by the steric hindrance of 2,6-dihexyloxybenzene units. The thermal behaviors were investigated with temperature-controlled polarizing optical microscopy, differential scanning calorimetry, powder X-ray diffraction, and absorption spectral analyses. Pc 1, having C4h molecular symmetry, organized into a lamellar structure containing lateral assemblies of Pc rings. In contrast, the other Pc 2 revealed the formation of metastable crystalline phases, including disordered stacks of Pcs due to rapid cooling from a melted liquid.


2000 ◽  
Vol 15 (7) ◽  
pp. 1617-1621 ◽  
Author(s):  
Jan Schroers ◽  
Konrad Samwer ◽  
Frigyes Szuecs ◽  
William L. Johnson

The reaction of the bulk glass forming alloy Zr41Ti14Cu12Ni10Be23 (Vit 1) with W, Ta, Mo, AlN, Al2O3, Si, graphite, and amorphous carbon was investigated. Vit 1 samples were melted and subsequently solidified after different processing times on discs of the different materials. Sessile drop examinations of the macroscopic wetting of Vit 1 on the discs as a function of temperature were carried out in situ with a digital optical camera. The reactions at the interfaces between the Vit 1 sample and the different disc materials were investigated with an electron microprobe. The structure and thermal stability of the processed Vit 1 samples were examined by x-ray diffraction and differential scanning calorimetry. The results are discussed in terms of possible applications for composite materials.


DYNA ◽  
2019 ◽  
Vol 86 (211) ◽  
pp. 278-287
Author(s):  
Javier Alberto Olarte Torres ◽  
María Cristina Cifuentes Arcila ◽  
Harvey Andrés Suárez Moreno

This paper presents the results obtained from the synthesis and morphological characterization of different magnetite samples:  La0.67-x Prx Ca0.33 MnO3.LaMn1-x Cox O3 and LaMn1-x Nix O3 at 0.13 ≤ 𝑥𝑥 ≤ 0.67 produced by a solid-state reaction mechanism and 𝐿𝐿𝐿𝐿𝑀𝑀𝑀𝑀1−𝑥𝑥(𝐶𝐶𝐶𝐶/𝑁𝑁𝑁𝑁)𝑥𝑥𝑂𝑂3 at 0.0 ≤ 𝑥𝑥 ≤ 0.5 produced by the sol-gel method. These samples were characterized using X-ray diffraction spectroscopy and by measuring electric resistivity and magnetic susceptibility which were carried out as a function of temperature. Notably, the effects of strain and compressive strength on the lattices of magnetite samples were highly dependent on the concentration of 𝑃𝑃𝑟𝑟, 𝐶𝐶𝐶𝐶, and 𝑁𝑁𝑁𝑁. Moreover, the transition temperatures of metal-insulator and ferromagnetic-paramagnetic phases also largely depend on these strength effects, e.g., at higher concentrations of 𝑃𝑃𝑟𝑟, effects of increased strain strength were observed, relocating the shifts of ferromagnetic-paramagnetic transitions to lower temperatures. On the other hand, effects of increased compressive strength were observed at higher concentrations of 𝑁𝑁𝑁𝑁 and 𝐶𝐶𝐶𝐶, relocating the shifts of ferromagnetic-paramagnetic and metal-insulator transitions to higher temperatures.


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