Reaction/crystallization kinetics studied via in situ XRD: experimental conditions versus methods of kinetic analysis

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F00216275%3A25310%2F19%3A39915585" target="_blank" >RIV/00216275:25310/19:39915585 - isvavai.cz</a>

Výsledek na webu

<a href="https://www.tandfonline.com/doi/abs/10.1080/14786435.2019.1648899?journalCode=tphm20" target="_blank" >https://www.tandfonline.com/doi/abs/10.1080/14786435.2019.1648899?journalCode=tphm20</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1080/14786435.2019.1648899" target="_blank" >10.1080/14786435.2019.1648899</a>

Jazyk výsledku

angličtina

Název v původním jazyce

Reaction/crystallization kinetics studied via in situ XRD: experimental conditions versus methods of kinetic analysis

Popis výsledku v původním jazyce

Theoretically simulated kinetic data were used to evaluate the errors associated with the common issue of evaluating the in situ non-isothermal X-ray diffraction data, where the complex multi-step temperature program (alternating the non-isothermal heating steps with isothermal steps during which the diffraction patterns are collected) is for the purposes of evaluation replaced by a simple non-isothermal heating performed at the reduced/effective heating rate. The kinetic analysis has shown that, in general, best results are provided by the non-linear optimisation methods simultaneously evaluating the data-curves obtained for all the different heating rates. For the nucleation growth (KMJMA) kinetics the distortive influence of the temperature program parameters increases as follows: heating rate during non-isothermal segments &lt; duration of the isothermal segment &lt; temperature interval between the isothermal segments. The non-optimisation methods of kinetic analysis (integral isoconversional methods for evaluation of activation energy E and master plots for determining the appropriate kinetic model) were found to perform inaccurately, with large degree of randomness based on the selection of starting temperature, and are not recommended for evaluation of the in situ XRD data - the only exception seem to be the differential isoconversional methods that provided accurate E values. Generalisation of the present conclusions for all KMJMA processes is suggested and discussed.

Název v anglickém jazyce

Reaction/crystallization kinetics studied via in situ XRD: experimental conditions versus methods of kinetic analysis

Popis výsledku anglicky

Theoretically simulated kinetic data were used to evaluate the errors associated with the common issue of evaluating the in situ non-isothermal X-ray diffraction data, where the complex multi-step temperature program (alternating the non-isothermal heating steps with isothermal steps during which the diffraction patterns are collected) is for the purposes of evaluation replaced by a simple non-isothermal heating performed at the reduced/effective heating rate. The kinetic analysis has shown that, in general, best results are provided by the non-linear optimisation methods simultaneously evaluating the data-curves obtained for all the different heating rates. For the nucleation growth (KMJMA) kinetics the distortive influence of the temperature program parameters increases as follows: heating rate during non-isothermal segments &lt; duration of the isothermal segment &lt; temperature interval between the isothermal segments. The non-optimisation methods of kinetic analysis (integral isoconversional methods for evaluation of activation energy E and master plots for determining the appropriate kinetic model) were found to perform inaccurately, with large degree of randomness based on the selection of starting temperature, and are not recommended for evaluation of the in situ XRD data - the only exception seem to be the differential isoconversional methods that provided accurate E values. Generalisation of the present conclusions for all KMJMA processes is suggested and discussed.

Druh

J_imp - Článek v periodiku v databázi Web of Science

CEP obor

—

OECD FORD obor

20501 - Materials engineering

Projekt

<a href="/cs/project/GA17-11753S" target="_blank" >GA17-11753S: Kinetická analýza komplexních fyzikálně chemických procesů</a><br>

Návaznosti

P - Projekt vyzkumu a vyvoje financovany z verejnych zdroju (s odkazem do CEP)

Rok uplatnění

2019

Kód důvěrnosti údajů

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Název periodika

Philosophical Magazine

ISSN

1478-6435

e-ISSN

—

Svazek periodika

99

Číslo periodika v rámci svazku

23

Stát vydavatele periodika

GB - Spojené království Velké Británie a Severního Irska

Počet stran výsledku

16

Strana od-do

2941-2956

Kód UT WoS článku

000481136000001

EID výsledku v databázi Scopus

2-s2.0-85070263964