Insights into the thermal decomposition of organometallic compound ferrocene carboxaldehyde as precursor for hematite nanoparticles synthesis

Chakraborty, Meenakshi; Dey, Anubha; Bhattacharjee, Ashis

doi:10.1515/zpch-2021-3175

Cited by 5 publications

(17 citation statements)

References 65 publications

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“…The kinetic study of a thermal solid-state reaction, in general, assumes that the rate equation can be expressed as the product of two distinct functions, k ( T ) and f (α) so that dα normald t = k ( T ) f ( α ) = A 0.25em exp ( E / R T ) f ( α ) where k ( T ) is the Arrhenius rate constant, f (α) is the differential conversion function, E is the activation energy, A is the reaction rate, and R is the universal gas constant. In the case of a nonisothermal reaction under constant heating rate (say, β = normald T normald t ), eq can be expressed as: β dα normald T = A f ( α ) 0.25em exp ( − E R T ) …”

Section: Experimental and Analytical Methodsmentioning

confidence: 99%

“…Parameters. The kinetic study of a thermal solid-state reaction, in general, assumes that the rate equation can be expressed as the product of two distinct functions, k(T) and f(α) 14 so that…”

Section: Computation Of Kineticmentioning

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%

“…Model-fitting techniques have a number of flaws, including an inability to accurately estimate the right reaction model and to depict the multistep kinetics and intricacy of solid-state reactions . Unlike model-fitting techniques, model-free methods of kinetic analysis can prevent inaccuracies associated with the selection of reaction models . Model-free techniques are only concerned with evaluating the activation energy over a broad range of temperatures and the extent of mass conversions from thermogravimetric data obtained at a minimum of three distinct heating rates.…”

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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