Thermal Analysis on Dehydroxylation of Sol-Gel Derived Zinc Doped Calcium Phosphate Powders

2015 ◽  
Vol 1115 ◽  
pp. 353-356
Author(s):  
Gunawan ◽  
I. Sopyan

The dehydroxylation of Zn free and 4 mol% Zn CaP powder was investigated using thermogravimetric analysis over the range of room temperature to 1200 °C. The kinetic result of dehydroxylation of Zn free and 4 mol% Zn CaP was calculated by means of the Ozawa–Flynn–Wall method. The XRD result indicated that the amount of Zn incorporated in HA lattice influences the phase stability of HA as it decreases with an increase in Zn concentration. According to calculated activation energy and conversion degree, the kinetics of HA dehydroxylation was identified, which included four successive conversion stages kinetically controlled by different rate-controlling processes. The dehydroxylation analysis of TG/DTG data show that Zn incorporation in HA lattice influences the phase stability of HA.

2021 ◽  
pp. 009524432110203
Author(s):  
Sudhir Bafna

It is often necessary to assess the effect of aging at room temperature over years/decades for hardware containing elastomeric components such as oring seals or shock isolators. In order to determine this effect, accelerated oven aging at elevated temperatures is pursued. When doing so, it is vital that the degradation mechanism still be representative of that prevalent at room temperature. This places an upper limit on the elevated oven temperature, which in turn, increases the dwell time in the oven. As a result, the oven dwell time can run into months, if not years, something that is not realistically feasible due to resource/schedule constraints in industry. Measuring activation energy (Ea) of elastomer aging by test methods such as tensile strength or elongation, compression set, modulus, oxygen consumption, etc. is expensive and time consuming. Use of kinetics of weight loss by ThermoGravimetric Analysis (TGA) using the Ozawa/Flynn/Wall method per ASTM E1641 is an attractive option (especially due to the availability of commercial instrumentation with software to make the required measurements and calculations) and is widely used. There is no fundamental scientific reason why the kinetics of weight loss at elevated temperatures should correlate to the kinetics of loss of mechanical properties over years/decades at room temperature. Ea obtained by high temperature weight loss is almost always significantly higher than that obtained by measurements of mechanical properties or oxygen consumption over extended periods at much lower temperatures. In this paper, data on five different elastomer types (butyl, nitrile, EPDM, polychloroprene and fluorocarbon) are presented to prove that point. Thus, use of Ea determined by weight loss by TGA tends to give unrealistically high values, which in turn, will lead to incorrectly high predictions of storage life at room temperature.


2020 ◽  
Vol 21 (11) ◽  
pp. 3785 ◽  
Author(s):  
Areej A. Eskandrani ◽  
Shimaa M. Ali ◽  
Hibah M. Al-Otaibi

The catalytic activity of Sr2PdO3, prepared through the sol-gel citrate-combustion method for the oxygen evolution reaction (OER) in a 0.1 M HClO4 solution, was investigated. The electrocatalytic activity of Sr2PdO3 toward OER was assessed via the anodic potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). The glassy carbon modified Sr2PdO3 (GC/Sr2PdO3) electrode exhibited a higher electrocatalytic activity, by about 50 times, in comparison to the unmodified electrode. The order of the reaction was close to unity, which indicates that the adsorption of the hydroxyl groups is a fast step. The calculated activation energy was 21.6 kJ.mol−1, which can be considered a low value in evaluation with those of the reported OER electrocatalysts. The Sr2PdO3 perovskite portrayed a high catalyst stability without any probability of catalyst poisoning. These results encourage the use of Sr2PdO3 as a candidate electrocatalyst for water splitting reactions.


Author(s):  
Ivan Hrušovský ◽  
Peter Rantuch ◽  
Jozef Martinka ◽  
Simona Dzíbelová

Abstract The decomposition stages of spruce wood sawdust were analyzed by means of sequential differential calorimetry. Two stages of decomposition were identified and activation energy of one stage was calculated using the Kissinger method. The DTA was conducted by means of SEDEX safety calorimeter. Sample was analyzed under three heating rates of 10, 20 and 45 °C/h in temperature range from room temperature to 400 °C. The calculated activation energy for the last and most clear decomposition peak was 122.63 KJ/mol. The results are comparable with the data calculated by J.V. Rissanen et al., who calculated activation energy for Spruce hemicellulose as 120 KJ/mol.


2013 ◽  
Vol 2013 ◽  
pp. 1-11 ◽  
Author(s):  
Lhaj Hachemi Omari ◽  
Salaheddine Sayouri

Polycrystalline perovskite nanomaterials (Pb0.88La0.12)(FexTi1-x)0.97O3 were prepared by sol-gel reaction method. The crystal structure examined by X-ray powder diffraction indicates that the material was single phase with pseudocubic structure. EDX and SEM studies were carried out in order to evaluate the quality and purity of the compounds. The crystal symmetry, space group, and unit cell dimensions were determined from Cell-Ref software, whereas crystallite size was estimated from Scherrer’s formula. A correlation between grain size and diffuse character for the samples has been observed. Dielectric studies exhibit a diffuse phase transition characterized by a strong temperature and frequency dispersion of the permittivity and a relaxor behaviour. We have observed that dielectric constant decreases and ac conductivity increases with the frequency. The dielectric relaxation has been modeled using the Curie-Weiss and modified Curie-Weiss laws. The calculated activation energy Ea for x=1% and 3% was between 0.91–2.1 eV and 0.425–1.08 eV, respectively. The relaxation times were estimated from the Arrhenius law.


2008 ◽  
Vol 40 (3) ◽  
pp. 263-270 ◽  
Author(s):  
D. Bucevac ◽  
S. Boskovic ◽  
B. Matovic

The ?-? phase transformation in Si3N4 was studied for seeded samples using an Y2O3-Al2O3 mixture as a sintering aid. The concentration of ?-seeds varied from 0 to 5 wt.%. The results showed that ?-? phase transformation followed the first-order reaction. The calculated activation energy for seeded samples was in the range from 348 to 378 KJ/mol, indicating boundary reaction as the rate limiting step.


Author(s):  
Harry A. Atwater ◽  
C.M. Yang ◽  
K.V. Shcheglov

Studies of the initial stages of nucleation of silicon and germanium have yielded insights that point the way to achievement of engineering control over crystal size evolution at the nanometer scale. In addition to their importance in understanding fundamental issues in nucleation, these studies are relevant to efforts to (i) control the size distributions of silicon and germanium “quantum dots𠇍, which will in turn enable control of the optical properties of these materials, (ii) and control the kinetics of crystallization of amorphous silicon and germanium films on amorphous insulating substrates so as to, e.g., produce crystalline grains of essentially arbitrary size.Ge quantum dot nanocrystals with average sizes between 2 nm and 9 nm were formed by room temperature ion implantation into SiO2, followed by precipitation during thermal anneals at temperatures between 30°C and 1200°C[1]. Surprisingly, it was found that Ge nanocrystal nucleation occurs at room temperature as shown in Fig. 1, and that subsequent microstructural evolution occurred via coarsening of the initial distribution.


1977 ◽  
Vol 16 (01) ◽  
pp. 30-35 ◽  
Author(s):  
N. Agha ◽  
R. B. R. Persson

SummaryGelchromatography column scanning has been used to study the fractions of 99mTc-pertechnetate, 99mTcchelate and reduced hydrolyzed 99mTc in preparations of 99mTc-EDTA(Sn) and 99mTc-DTPA(Sn). The labelling yield of 99mTc-EDTA(Sn) chelate was as high as 90—95% when 100 μmol EDTA · H4 and 0.5 (Amol SnCl2 was incubated with 10 ml 99mTceluate for 30—60 min at room temperature. The study of the influence of the pH-value on the fraction of 99mTc-EDTA shows that pH 2.8—2.9 gave the best labelling yield. In a comparative study of the labelling kinetics of 99mTc-EDTA(Sn) and 99mTc- DTPA(Sn) at different temperatures (7, 22 and 37°C), no significant influence on the reduction step was found. The rate constant for complex formation, however, increased more rapidly with increased temperature for 99mTc-DTPA(Sn). At room temperature only a few minutes was required to achieve a high labelling yield with 99mTc-DTPA(Sn) whereas about 60 min was required for 99mTc-EDTA(Sn). Comparative biokinetic studies in rabbits showed that the maximum activity in kidneys is achieved after 12 min with 99mTc-EDTA(Sn) but already after 6 min with 99mTc-DTPA(Sn). The long-term disappearance of 99mTc-DTPA(Sn) from the kidneys is about five times faster than that for 99mTc-EDTA(Sn).


1993 ◽  
Vol 329 ◽  
Author(s):  
Michael Canva ◽  
Patrick Georges ◽  
Jean-Fran^ois Perelgritz ◽  
Alain Brun ◽  
Fréddric Chaput ◽  
...  

AbstractPhotoresistant laser dyes were trapped in silica based xerogel host matrices to obtain solid state tunable lasers. For this purpose very dense xerogel samples with improved chemical and physical properties were prepared at room temperature by the sol-gel technology. The as-prepared materials were polished to obtain optical quality surfaces and were used as new lasing media.Lasing action of such different dyes as rhodamine, perylene and pyrromethene doping dense sol-gel matrices was demonstrated. Efficiencies of 30 % or lifetimes of more than 100,000 shots were achieved with different new ≤dye dopant/host matrix≥ couples. Their different performances are reviewed and discussed.


2009 ◽  
Vol 59 (12) ◽  
Author(s):  
Mihai Contineanu ◽  
iulia Contineanu ◽  
Ana Neacsu ◽  
Stefan Perisanu

The radiolysis of the isomers L-, D- and DL- of the aspartic acid, in solid polycrystalline state, was investigated at room temperature. The analysis of their ESR spectra indicated the formation of at least two radicalic entities. The radical, identified as R3, resulting from the deamination of the acid, exhibits the highest concentration and thermal resistance. Possible mechanisms of formation of three radical species are suggested, based also on literature data. The kinetics of the disappearance of radical R3 indicated a complex mechanism. Three possible variants were suggested for this mechanism.


Author(s):  
Mohsen Nikoorazm ◽  
Maryam Khanmoradi ◽  
Masoumeh Sayadian

Introduction:: MCM-41 was synthesized using the sol-gel method. Then two new transition metal complexes of Nickel (II) and Vanadium (IV), were synthesized by immobilization of adenine (6-aminopurine) into MCM-41 mesoporous. The compounds have been characterized by XRD, TGA, SEM, AAS and FT-IR spectral studies. Using these catalysts provided an efficient and enantioselective procedure for oxidation of sulfides to sulfoxides and oxidative coupling of thiols to their corresponding disulfides using hydrogen peroxide at room temperature. Materials and Methods:: To a solution of sulfide or thiol (1 mmol) and H2O2 (5 mmol), a determined amount of the catalyst was added. The reaction mixture was stirred at room temperature for the specific time under solvent free conditions. The progress of the reaction was monitored by TLC using n-hexane: acetone (8:2). Afterwards, the catalyst was removed from the reaction mixture by centrifugation and, then, washed with dichloromethane in order to give the pure products. Results:: All the products were obtained in excellent yields and short reaction times indicating the high activity of the synthesized catalysts. Besides, the catalysts can be recovered and reused for several runs without significant loss in their catalytic activity. Conclusion:: These catalytic systems furnish the products very quickly with excellent yields and VO-6AP-MCM-41 shows high catalytic activity compared to Ni-6AP-MCM-41.


Sign in / Sign up

Export Citation Format

Share Document