scholarly journals Heating rate dependence of anatase to rutile transformation

2016 ◽  
Vol 10 (4) ◽  
pp. 235-241 ◽  
Author(s):  
Pietro Galizia ◽  
Giovanni Maizza ◽  
Carmen Galassi

Commercial titania powders were calcined in order to investigate the influence of the heating history on the thermally stable phase (rutile). Temperatures from 620 to 700?C and heating rates from 50 to 300?C/h were used in order to evaluate their influence on the kinetics of transformation and microstructure evolution. The quantitative analysis of anatase-rutile mixtures based on X-ray diffraction intensities was performed. The results were plotted as cumulative transformation rate vs. cumulative coarsening rate in order to address the heating history of the anatase to rutile transformation. As the main result it was found that the amount of anatase transformed into rutile increases with increasing heating rate at fixed soaking time and temperature of calcination. Through linear extrapolation of experimental data obtained from the calcined commercial titania Degussa P25, it was found that 83 nm for the rutile crystallite size is the lowest limit needed for getting 100% of rutile powders. A substantial improvement in the anatase to rutile kinetic transformation was achieved after pressing the starting powders in order to exploit the interface nucleation.

Author(s):  
A. Leineweber ◽  
M. Löffler ◽  
S. Martin

Abstract Cu6Sn5 intermetallic occurs in the form of differently ordered phases η, η′ and η′′. In solder joints, this intermetallic can undergo changes in composition and the state of order without or while interacting with excess Cu and excess Sn in the system, potentially giving rise to detrimental changes in the mechanical properties of the solder. In order to study such processes in fundamental detail and to get more detailed information about the metastable and stable phase equilibria, model alloys consisting of Cu3Sn + Cu6Sn5 as well as Cu6Sn5 + Sn-rich melt were heat treated. Powder x-ray diffraction and scanning electron microscopy supplemented by electron backscatter diffraction were used to investigate the structural and microstructural changes. It was shown that Sn-poor η can increase its Sn content by Cu3Sn precipitation at grain boundaries or by uptake of Sn from the Sn-rich melt. From the kinetics of the former process at 513 K and the grain size of the η phase, we obtained an interdiffusion coefficient in η of (3 ± 1) × 10−16 m2 s−1. Comparison of this value with literature data implies that this value reflects pure volume (inter)diffusion, while Cu6Sn5 growth at low temperature is typically strongly influenced by grain-boundary diffusion. These investigations also confirm that η′′ forming below a composition-dependent transus temperature gradually enriches in Sn content, confirming that Sn-poor η′′ is metastable against decomposition into Cu3Sn and more Sn-rich η or (at lower temperatures) η′. Graphic Abstract


2020 ◽  
Vol 39 (2) ◽  
pp. 227
Author(s):  
Adnan Kurt ◽  
Hacer Andan ◽  
Murat Koca

A new conjugated polymer containing a bithiazole group is prepared by the polycondensation of 2,2'-diamino-4,4'-bithiazole and terephthaldialdehyde in the presence of glacial acetic acid. The kinetics of thermal degradation of the new polymer are investigated by thermogravimetric analysis at different heating rates. The temperature corresponding to the maximum rate loss shifts to higher temperatures with increasing heating rate. The thermal decomposition activation energies of the conjugated polymer in a conversion range of 3–15 % are 288.4 and 281.1 kJ/mol by the Flynn–Wall–Ozawa and Kissinger methods, respectively. The Horowitz–Metzger method shows that the thermodegradation mechanism of the conjugated polymer proceeds over a three-dimensional diffusion type deceleration D3 mechanism. The optimum heating rate is 20 ºC/min.


2014 ◽  
Vol 32 (3) ◽  
pp. 385-390
Author(s):  
Aysel Kantürk Figen ◽  
Bilge Coşkuner ◽  
Sabriye Pişkin

AbstractIn the present study, hydrogen desorption properties of magnesium hydride (MgH2) synthesized from modified waste magnesium chips (WMC) were investigated. MgH2 was synthesized by hydrogenation of modified waste magnesium at 320 °C for 90 min under a pressure of 6 × 106 Pa. The modified waste magnesium was prepared by mixing waste magnesium with tetrahydrofuran (THF) and NaCl additions, applying mechanical milling. Next, it was investigated by X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and Brunauer-Emmett-Teller (BET) techniques in order to characterize its structural properties. Hydrogen desorption properties were determined by differential scanning calorimetry (DSC) under nitrogen atmosphere at different heating rates (5, 10, and 15 °C/min). Doyle and Kissenger non-isothermal kinetic models were applied to calculate energy (Ea) values, which were found equal to 254.68 kJ/mol and 255.88 kJ/mol, respectively.


1991 ◽  
Vol 31 (1) ◽  
pp. 325 ◽  
Author(s):  
R. Alexander ◽  
P.G. Kralert ◽  
R. Marzi ◽  
R.I. Kagi ◽  
E J. Evans

The ester content in kerogen is depleted as sediment maturation progresses in a process which has been shown to correlate with change in the carbon preference index (CPI) of the associated soluble organic matter. We have carried out accurate laboratory measurements of the kinetics of the reaction which causes ester depletion in sediments, and we show how this information can be used to assess the thermal history of sediments. Two wells were selected, Grunter-1 and Volador-1, to provide samples from the Latrobe Group in the Gippsland Basin. The CPI values were measured to assess the extent of reaction at points down each well, and these values were then used with the kinetic parameters for the ester depletion process to obtain thermal histories which are consistent with the available maturity information.This treatment enabled the heat flow from 50 Ma to the present to be assessed and it suggests that at both locations a constant low heat flow during the Gippsland stable phase was followed by a gradual increase from the beginning of the Miocene to present-day values.


2014 ◽  
Vol 953-954 ◽  
pp. 261-266
Author(s):  
Dong Yu Chen ◽  
Yan Qing Hu ◽  
Qing Yu Liu

To study the influences of the acid-washing on the characteristics of soybean stalk pyrolysis , and search the high-efficiency catalyst for biomass pyrolysis, pyrolysis experiments of soybean stalk pretreated by 0.1mol/L HCl acid solution were performed by nonisothermal thermogravimetric analysis (TGA) at five different heating rates. The results showed the pyrolysis process of HCl-washed soybean stalk can be separated into four stages (water loss, depolymeri-zation and vitrification, thermal decomposition, and carbonization). At the same heating rate, the maximum pyrolysis rate of HCl-washed is larger than untreated soybean stalk, but the corresponding temperature is higher. All the DTG (differential thermogravimetric) curveas appear a smaller shoulder peak respectively. With the heating rate increasing, the main pyrolysis zone of the TG (thermogravimetric) and DTG curves move to the high-temperature direction, and the maximum pyrolysis rate and its corresponding temperature increase too. HCl-wahsed makes the weight loss rate of the final temperature increase 5% approximately. The value area of activation energy of the main pyrolysis area is 140.19~174.59 kJ/mol calculated by the method of Ozawa. The Šatava method inferred the most possible mechanism function of HCl-wahsed soybean stalk is Zhuralev-Lesakin-Tempelman equation, which is three-dimensional diffusion.


2021 ◽  
Vol 9 ◽  
Author(s):  
Stefan Pielsticker ◽  
Benjamin Gövert ◽  
Kentaro Umeki ◽  
Reinhold Kneer

Biomass is a complex material mainly composed of the three lignocellulosic components: cellulose, hemicellulose and lignin. The different molecular structures of the individual components result in various decomposition mechanisms during the pyrolysis process. To understand the underlying reactions in more detail, the individual components can be extracted from the biomass and can then be investigated separately. In this work, the pyrolysis kinetics of extracted and purified cellulose, hemicellulose and lignin are examined experimentally in a small-scale fluidized bed reactor (FBR) under N2 pyrolysis conditions. The FBR provides high particle heating rates (approx. 104 K/s) at medium temperatures (573–973 K) with unlimited reaction time and thus complements typically used thermogravimetric analyzers (TGA, low heating rate) and drop tube reactors (high temperature and heating rate). Based on the time-dependent gas concentrations of 22 species, the release rates of these species as well as the overall rate of volatiles released are calculated. A single first-order (SFOR) reaction model and a 2-step model combined with Arrhenius kinetics are calibrated for all three components individually. Considering FBR and additional TGA experiments, different reaction regimes with different activation energies could be identified. By using dimensionless pyrolysis numbers, limits due to reaction kinetics and heat transfer could be determined. The evaluation of the overall model performance revealed model predictions within the ±2σ standard deviation band for cellulose and hemicellulose. For lignin, only the 2-step model gave satisfying results. Modifications to the SFOR model (yield restriction to primary pyrolysis peak or the assumption of distributed reactivity) were found to be promising approaches for the description of flash pyrolysis behavior, which will be further investigated in the future.


2021 ◽  
Author(s):  
Mehmet Isik ◽  
Serdar Delice ◽  
Nizami M Gasanly

Abstract Bi12SiO20 (BSO) single crystal belongs to the sillenite semiconducting family known as defective compounds. The present paper investigates the defect centers in BSO grown by Czochralski method by means of thermally stimulated current (TSC) measurements performed in the 10-260 K range. The TSC glow curve obtained at heating rate of β = 0.1 K/s presented several peaks associated with intrinsic defect centers. The activation energies of defect centers were revealed as 0.09, 0.15, 0.18, 0.22, 0.34, 0.70 and 0.82 eV accomplishing the curve fit analyses method. The peak maximum temperatures and orders of kinetics of each deconvoluted peak were also determined as an outcome of fitting process. TSC experiments were expanded by making the measurements at various heating rates between 0.1 and 0.3 K/s to get information about the heating rate dependent peak parameters.


1985 ◽  
Vol 29 ◽  
pp. 315-322 ◽  
Author(s):  
C. E. Crowder ◽  
S. Wood ◽  
B. G. Landes ◽  
R. A. Newman ◽  
J. A. Blazy ◽  
...  

Over the past 25 years, numerous studies of polymers utilizing both X-ray diffraction (XRD) and differential scanning calorimetry (DSC) have been reported in the literature. These studies have suffered because the two techniques must be performed on separate samples and under conditions that are often dissimilar. By combining the two techniques into one instrument, typical problems encountered with variations in sample preparation and thermal and atmospheric environment are eliminated. This is quite important in the study of polymers since one must match not only temperatures between the two techniques, but also heating rates as well. Matched thermal conditions are necessary because polymer properties such as crystallinity and crystallite size depend on both the temperature and thermal history of the sample under study.


2014 ◽  
Vol 67 (1) ◽  
pp. 61-66 ◽  
Author(s):  
Maximiano Maicon Batista Lopes ◽  
André Barros Cota

The austenite formation under isochronal conditions in Nb microalloyed low carbon steel was studied by means of dilatometric analysis and the data was adjusted to the Johnson-Mehl-Avrami-Kolmogorov (JMAK) equation, for different heating rates and for three initial microstructures. It was shown that the kinetics of austenitization of a pearlite+ferrite structure is faster than that of martensite (tempered martensite) at a heating rate of 0.1ºC/s. For heating rates higher than 0.1ºC/s, the kinetics of austenitization of a martensite structure is faster than of pearlite+ferrite one. The K parameter of the JMAK equation increases with the heating rate for the three previous microstructures and it is greater for the initial microstructure composed of ferrite+pearlite. At lower heating rates, the formation of austenite in this steel is controlled by carbon diffusion, independently of the initial microstructure. At higher heating rates, the formation of austenite from an initial microstructure composed of pearlite and ferrite is controlled by interface-controlled transformation.


2012 ◽  
Vol 727-728 ◽  
pp. 721-726 ◽  
Author(s):  
Lisiane Navarro de Lima Santana ◽  
Bartolomeu Jorge da Silva ◽  
Wherllyson Patrício Gonçalves ◽  
Juliana Melo Cartaxo ◽  
Bruna Silveira Lira ◽  
...  

In the ceramic industry, the firing is one of the main stages of the production process. There are two heating rates prevailing at this stage: low heating rate (long residence time) and high heating rate (fast residence time), the low rate is more used in traditional ceramics. This study aims to evaluate the influence of firing conditions on technological properties of three compositions of clay, used in the manufacture of red ceramic products. Initially, the mixtures were characterized subsequently were extruded, dried and submitted to firing at temperatures at 900 and 1000 °C with heating rates of 1, 2, 5, 15, 20 and 30 °C/min. The crystalline evolution of the different samples was analyzed using X-ray diffraction and the technological properties were determined. For the mechanical resistance, it was not observed significant change with the increase of the temperature and heat rate


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