Thermal transformation of 1-(ferrocenyl)ethanol to iron oxide nanoparticles based on reaction atmosphere: analysis of the decomposition reaction using non-isothermal thermogravimetry

Chakraborty, Meenakshi; Kundu, Sukumar; Das, Bratati; Bhattacharjee, A.

doi:10.1007/s10973-023-12306-x

Cited by 4 publications

(18 citation statements)

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“…The Arrhenius parameters of process i are denoted by A i , E α, i , f i (α i ), respectively. α ( = m i − m t m i − m f ) represents the extent of conversion of the overall process, where m i is the initial mass, m f is the final mass, and m t is mass at any instant of reaction . To separate the individual peaks from the overall TG profile, Fraser–Suzuki (FS) function is used, which produces a very good fitting result, defined as dα normald T = ∑ i = 1 n d α i d T = ∑ i = 1 n ( h i exp true[ prefix− ln nobreak0em.25em⁡ 2 s i 2 true[ ln ( 1 + 2 s i ( T − P i ) w i ) true] 2 true] ) where dα normald T is the conversion rate of the overall process, ...…”

Section: Experimental and Analytical Methodsmentioning

confidence: 99%

“…The changes in entropy (Δ S ), enthalpy (Δ H ), and Gibbs free energy (Δ G ) for the activated complex formation during the thermal decomposition process can be calculated using the following relation: normalΔ S = R 0.25em ln ( A α h e χ k B T p ) 0.25em normalΔ H = E α − R T normalp and normalΔ G = normalΔ H − T normalp normalΔ S where e = 2.7183 (base of natural logarithm); χ is the transition factor; k B is the Boltzmann constant; h is Plank’s constant, and T p is the peak temperature of the differential TG curve at the corresponding step.…”

Section: Experimental and Analytical Methodsmentioning

confidence: 99%

“…The Arrhenius parameters of process i are denoted by A i , E α, i , f i (α i ), respectively. represents the extent of conversion of the overall process, where m i is the initial mass, m f is the final mass, and m t is mass at any instant of reaction . To separate the individual peaks from the overall TG profile, Fraser–Suzuki (FS) function is used, which produces a very good fitting result, defined as where is the conversion rate of the overall process, h i , p i , s i , and w i are the fit parameters corresponding to peak amplitude, position, asymmetry, and half-width of the i th thpeak, respectively .…”

Section: Experimental and Analytical Methodsmentioning

confidence: 99%

“…16 Unlike model-fitting techniques, model-free methods of kinetic analysis can prevent inaccuracies associated with the selection of reaction models. 14 Model-free techniques are only concerned with evaluating the activation energy over a broad range of temperatures and the extent of mass conversions 13 from thermogravimetric data obtained at a minimum of three distinct heating rates. There are two major categories of modelfree methods: differential methods and integral methods.…”

Section: Introductionmentioning

confidence: 99%

“…The kinetic theory of thermal analysis is aptly applied to study the process of thermal reaction and formation of new material. Thermogravimetric analysis is a well-known method to investigate the solid-state thermal reactions, which reflects the change of sample mass upon heating. , The most popular method for thermal study of materials is nonisothermal thermogravimetry (TG), which needs to obtain the TG profiles of the powdered sample at different heating rates. The analysis of the TG curves based on the isoconversional protocol enables the estimation of the kinetic parameters (activation energy, mechanism function, and reaction rate) and the mechanism of the rate-controlled conversion process.…”

Section: Introductionmentioning

confidence: 99%

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Solid-State Reaction of Ferrocene Controlled by Co-Precursor and Reaction Atmosphere Leading to Hematite and Cohenite Nanomaterials: A Reaction Kinetic Study

Kundu,

Chakraborty,

Bhattacharjee

2023

J. Phys. Chem. C

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The present article investigates the thermal decomposition of ferrocene in the presence of oxalic acid dihydrate in oxidative and inert atmospheres. A mixture of ferrocene and oxalic acid dihydrate on thermal decomposition in O 2 and N 2 atmospheres produces hematite and cohenite nanomaterials, respectively. These decompositions are complex and reflected through multiple overlapped reaction steps in the thermogravimetry profiles, and peak deconvolution method is adopted to separate the reaction steps involved. It is found that the synthesis of hematite is a two-step process, while that of cohenite is a one-step process. Model-free integral isoconversional methods are adopted to estimate the values of activation energy for these thermal reactions. The most probable reaction mechanism and the reaction rate of thermal decomposition are determined by an intercept-based model fitting method. The reaction mechanism is found to be different for different steps. To verify the suitability of the adopted kinetic models, the experimental conversion curves are compared with the reversely constructed ones and the agreement is quite reasonable. The conversion dependence of thermodynamic parameters is obtained using the estimated kinetic parameters. Comparing the estimated values of the kinetic and thermodynamic parameters, the effect of the reaction atmosphere on the thermal decomposition process of ferrocene is realized. Utilizing the kinetic and thermodynamic parameters conversion-dependent nucleation rates of the reaction steps have been estimated. The present study describes how different nanomaterials of iron can be synthesized starting with the same precursor material, how the reaction (solid and gaseous) atmosphere affects the reaction profile and the residual material, and finally, how kinetic calculations help in understanding the solid state reaction process involved. This study suggests the use suitable combination of precursor, co-precursor, and gaseous reaction atmosphere for the solid-state thermal synthesis of iron-based nanoparticles using organo-iron compounds. The study also highlights the successful application of the peak-deconvolution method.

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