Iso-Conversional and Isokinetic Methods of Analysis of Non-Isothermal Crystallization in Ti50Cu20Ni30 Metallic Glass

2011 ◽  
Vol 171 ◽  
pp. 107-119
Author(s):  
Heena Dhurandhar ◽  
T. Lilly Shanker Rao ◽  
Kirit N. Lad ◽  
Arun Pratap

The crystallization kinetics of metallic glass Ti50Cu20Ni30 has been studied using Differential Scanning Calorimetry (DSC). The DSC thermograms have been analysed using the model-free isoconversional methods and model dependent isokinetic methods. The activation energy(E) for the crystallization process has been determined utilizing; (i) various linear integral isoconversional methods, namely, Ozawa-Flynn-Wall, Kissinger-Akahira-Sunose, Li Tang method (ii) linear differential isoconversional method and (iii) different isokinetic methods. In the present work, we intend to the determination of true value of E. The above methods are found to give consistent results for E.

2016 ◽  
Vol 701 ◽  
pp. 315-319
Author(s):  
Kevinilo P. Marquez ◽  
Rheo B. Lamorena-Lim

Analysis of the complex and variable nature of the chemical composition of asphalt has been a challenge to engineers and scientists, especially as a means to understand its behavior and suggest ways to improve its properties. In this study, the thermal behavior and the non-isothermal degradation kinetics were analyzed using the isoconversional methods, through Thermogravimetric analysis (TGA) and Differential Scanning Calorimetry (DSC). TGA and DSC data show gradual change in the mass of the material at increasing temperature, suggesting behavior typical of a homogenous mixture. Kinetic analysis from the TGA data using the Starink modification of the Kissinger-Akahira-Sunose Isoconversional method show an apparent increase in the magnitude of the activation energies at different conversion degree, which suggests a gradual change in the composition of the material at each successive conversion due to a single heat-promoted transformation of each of the components.


2011 ◽  
Vol 65 (6) ◽  
pp. 717-726 ◽  
Author(s):  
Mladjan Popovic ◽  
Jaroslava Budinski-Simendic ◽  
Mirjana Jovicic ◽  
Joszef Mursics ◽  
Milanka Djiporovic-Momcilovic ◽  
...  

Differential scanning calorimetry (DSC) was used to evaluate the curing kinetics of two commercial urea-formaldehyde (UF) adhesives having different formaldehyde to urea (F/U) ratio of 1.112 (UF1) and 1.086 (UF2). DSC measurements were done in dynamic scanning regime with heating rates of 5, 10, 15 and 20?C?min-1 in order to determine the activation energy for each adhesive. Obtained data were analyzed using isoconversional methods with application of Ozawa-Flynn-Wall and Kissinger-Akahira-Sunose kinetic models. In addition, different catalyst levels were tested at the heating rate of 10?C/min. Results showed that the adhesive with higher F/U ratio achieved higher activation energy, while having lower peak temperature of curing reaction. It was also noticed that the increase of catalyst level influenced the increase of reaction enthalpy of the adhesive with lower F/U ratio.


2018 ◽  
Vol 7 (1) ◽  
pp. 21-30 ◽  
Author(s):  
Norbert Halmen ◽  
Christoph Kugler ◽  
Eduard Kraus ◽  
Benjamin Baudrit ◽  
Thomas Hochrein ◽  
...  

Abstract. The degree of cross-linking and curing is one of the most important values concerning the quality of cross-linked polyethylene (PE-X) and the functionality of adhesives and resin-based components. Up to now, the measurement of this property has mostly been time-consuming and usually destructive. Within the shown work the feasibility of single-sided nuclear magnetic resonance (NMR) for the non-destructive determination of the degree of cross-linking and curing as process monitoring was investigated. First results indicate the possibility of distinguishing between PE-X samples with different degrees of cross-linking. The homogeneity of the samples and the curing kinetics of adhesives can also be monitored. The measurements show good agreement with reference tests (wet chemical analysis, differential scanning calorimetry, dielectric analysis). Furthermore, the influence of sample temperature on the characteristic relaxation times can be observed.


2020 ◽  
Vol 4 (2) ◽  
pp. 52
Author(s):  
Thaís Larissa do Amaral Montanheiro ◽  
Beatriz Rossi Canuto de Menezes ◽  
Larissa Stieven Montagna ◽  
Cesar Augusto Gonçalves Beatrice ◽  
Juliano Marini ◽  
...  

Carbon nanotubes (CNT)-reinforced polymeric composites are being studied as promising materials due to their enhanced properties. However, understanding the behavior of polymers during non-isothermal crystallization is important once the degree of crystallinity and crystallization processes are affected when nanoparticles are added to matrices. Usually, crystallization kinetics studies are performed using a model-fitting method, though the isoconversional method allows to obtain the kinetics parameter without assuming a crystallization model. Therefore, in this work, CNTs were oxidized (CNT-Ox) and functionalized with gamma-aminobutyric acid (GABA) (CNT-GB) and incorporated into a poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) matrix. The influence of the addition and functionalization of CNT in the crystallization kinetics of PHBV was evaluated using the isoconversional method with differential scanning calorimetry (DSC), and by polarized light optical microscopy (PLOM) and Shore D hardness. The incorporation and functionalization of CNT into PHBV matrix did not change the Šesták and Berggren crystallization model; however, the lowest activation energy was obtained for the composite produced with CNT-GB, suggesting a better dispersion into the PHBV matrix. PLOM and Shore D hardness confirmed the results obtained in the kinetics study, showing the smallest crystallite size for CNT-containing nanocomposites and the highest hardness value for the composite produced with CNT-GB.


2020 ◽  
Vol 4 (3) ◽  
pp. 111
Author(s):  
Zohre Karami ◽  
Seyed Mohammad Reza Paran ◽  
Poornima Vijayan P. ◽  
Mohammad Reza Ganjali ◽  
Maryam Jouyandeh ◽  
...  

Layered double hydroxide (LDH) minerals are promising candidates for developing polymer nanocomposites and the exchange of intercalating anions and metal ions in the LDH structure considerably affects their ultimate properties. Despite the fact that the synthesis of various kinds of LDHs has been the subject of numerous studies, the cure kinetics of LDH-based thermoset polymer composites has rarely been investigated. Herein, binary and ternary structures, including [Mg0.75 Al0.25 (OH)2]0.25+ [(CO32−)0.25/2∙m H2O]0.25−, [Mg0.75 Al0.25 (OH)2]0.25+ [(NO3−)0.25∙m H2O]0.25− and [Mg0.64 Zn0.11 Al0.25 (OH)2]0.25+ [(CO32−)0.25/2∙m H2O]0.25−, have been incorporated into epoxy to study the cure kinetics of the resulting nanocomposites by differential scanning calorimetry (DSC). Both integral and differential isoconversional methods serve to study the non-isothermal curing reactions of epoxy nanocomposites. The effects of carbonate and nitrate ions as intercalating agents on the cure kinetics are also discussed. The activation energy of cure (Eα) was calculated based on the Friedman and Kissinger–Akahira–Sunose (KAS) methods for epoxy/LDH nanocomposites. The order of autocatalytic reaction (m) for the epoxy/Mg-Al-NO3 (0.30 and 0.254 calculated by the Friedman and KAS methods, respectively) was smaller than that of the neat epoxy, which suggested a shift of the curing mechanism from an autocatalytic to noncatalytic reaction. Moreover, a higher frequency factor for the aforementioned nanocomposite suggests that the incorporation of Mg-Al-NO3 in the epoxy composite improved the curability of the epoxy. The results elucidate that the intercalating anions and the metal constituent of LDH significantly govern the cure kinetics of epoxy by the participation of nitrate anions in the epoxide ring-opening reaction.


2010 ◽  
Vol 160-162 ◽  
pp. 1712-1715
Author(s):  
Guang Heng Wang

The polymerization reaction kinetics of biodegradable polyurethane extended with soy protein isolate (SPI) with dibutyltin dilaurate (DBTDL) as the curing catalyst was studied by means of non-isothermal differential scanning calorimetry (DSC). Model-free methods, Kissinger method and Ozawa method, were applied for analyzing the DSC data. The Ea and lnA obtained from Kissinger method for catalyzed reaction between toluene diisocyanate (TDI) and Polyoxypropyleneglycol (PPG) are 60.80 kJ•mol-1 and 12.09, and for catalyzed reaction among TDI, PPG, and SPI they were 65.91 kJ•mol-1and 14.04. Similarly the Ea obtained from Ozawa method for catalyzed reaction between TDI and PPG and catalyzed reaction among TDI, PPG, and SPI were 63.49 kJ•mol-1 and 64.78 kJ•mol-1, respectively. The results showed that, the incorporation of a small amount of SPI into polyurethane did not affect the reaction kinetic strongly, but increases the reaction activation energy Ea and lnA.


Author(s):  
Dora Janovszky ◽  
Maria Sveda ◽  
Anna Sycheva ◽  
Ferenc Kristaly ◽  
Ferenc Zámborszky ◽  
...  

AbstractA remarkable number of scientific papers are available in the literature about the bulk amorphous alloys and metallic glasses. Today, DSC is an essential tool for amorphous alloys research and development, and of course for quality assurance. In many cases, users seek to examine the determination of only one or two properties, although much more information can be obtained from the measurements. The research involved structural relaxation, Curie temperature, glass temperature, crystallization, phase separation, nanocrystalline volume fraction, melting point and liquidus temperature determination subjects and kinetics of microstructural transformations induced by thermal treatment. We collected and present the information that can be obtained with this technique and draws the reader’s attention to some potential problems related to data interpretation.


Molecules ◽  
2020 ◽  
Vol 25 (12) ◽  
pp. 2813 ◽  
Author(s):  
Sergey Vyazovkin

The Kissinger method is an overwhelmingly popular way of estimating the activation energy of thermally stimulated processes studied by differential scanning calorimetry (DSC), differential thermal analysis (DTA), and derivative thermogravimetry (DTG). The simplicity of its use is offset considerably by the number of problems that result from underlying assumptions. The assumption of a first-order reaction introduces a certain evaluation error that may become very large when applying temperature programs other than linear heating. The assumption of heating is embedded in the final equation that makes the method inapplicable to any data obtained on cooling. The method yields a single activation energy in agreement with the assumption of single-step kinetics that creates a problem with the majority of applications. This is illustrated by applying the Kissinger method to some chemical reactions, crystallization, glass transition, and melting. In the cases when the isoconversional activation energy varies significantly, the Kissinger plots tend to be almost perfectly linear that means the method fails to detect the inherent complexity of the processes. It is stressed that the Kissinger method is never the best choice when one is looking for insights into the processes kinetics. Comparably simple isoconversional methods offer an insightful alternative.


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