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Role of ferrocene-derived iron species in the catalytic graphitization of novolak resins

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Abstract

Catalytic graphitization has been used since years, normally by heating from room temperature to 2227 or 3027 °C. Ferrocene was used to induce the graphitization in modified novolak phenolic resins synthesized in laboratory (PR). In this study, the intermediate carbon structures containing iron during the graphitization process, obtained after the different steps of heat treatment from 200 to 1000 °C, were identified concerning the oxidation states of iron and morphological and structural variations. The role of iron in these intermediate structures has not been fully evaluated yet by resonance and spectroscopy techniques; therefore, in this study, it will be discussed briefly. The following techniques were employed: X-ray powder diffraction (XRD), high-resolution transmission electron microscopy (HR-TEM), standard solid-state 13carbon nuclear magnetic resonance (solid-state 13C-NMR), 57Fe-Mössbauer and electron paramagnetic resonance (EPR) spectroscopies. In the material (PRFc) obtained by heat treatment for 5 h at 1000 °C, there were identified Fe2O3 nanocrystals, as well as Fe2O3, Fe3C and γ-iron present inside and outside of an onion-like hollow carbon structure. This structure of PRFc treated at 1000 °C has shown high efficiency in removing the pesticide atrazine (ATZ) in an aqueous medium and influenced the degradation mechanism of ATZ and the formation of atrazine-2-hydroxy (HAT).

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Acknowledgement

The authors would like to express their gratitude to Magnesita Refratários SA for the materials used in this study and the Federation for International Refractory Research and Education (FIRE), to the Laboratory of Nuclear Magnetic Resonance, Department of Chemistry-UFSCar, DEMa-UFSCar, Department of Ceramics-UFSCar, Federal University of Alfenas, Institute of Science and Technology, University of São Paulo, São Carlos Institute of Physics, CBPF-Brazilian Center for Research in Physics, Laboratory of Structural Characterization (LCE-DEMa/UFSCar) and LAMAV-UFSCar for their technical assistance in this study. In addition, E. Baggio Saitovitch acknowledges support from FAPERJ through several grants including Emeritus Professor Fellowship and Conselho Nacional de Desenvolvimento Científico e Tecnológico-Brasil (CNPq) for BPA and corresponding grants. This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior-Brasil (CAPES)-Finance Code 001. The authors thank the Federal University of Sao Carlos, Post Graduate Program in Materials Science and Engineering (PPGCEM) and CNPq (Process 168691/2017-5) for the financial assistance in disseminating this research.

Funding

The corresponding author (Carmen Greice Renda) was funded by Conselho Nacional de Desenvolvimento Científico e Tecnológico-Brasil-CNPq (Grant Number 168691/2017-5) and Coordenação de Aperfeiçoamento de Pessoal de Nível Superior-Brasil (CAPES)-Finance Code 001.

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  1. Federal University of São Carlos, Washington Luiz Highway, km 235, São Carlos, SP, 13565-905, Brazil

    Carmen Greice Renda, Leonardo Jose Dalla Costa, Alexandre José Gualdi, Tiago Venâncio, Ailton José Moreira & Alessandra de Almeida Lucas

  2. Institute of Science and Technology, Federal University of Alfenas, José A. Vilela Highway, 11999, BR 267, Km 533, Poços de Caldas, MG, 37715-400, Brazil

    Roberto Bertholdo & Gian Paulo Giovanni Freschi

  3. University of São Paulo, Institute of Physics of São Carlos, Trabalhador São Carlense Highway, 400, Parque Arnold Schimidt, São Carlos, SP, 13566-590, Brazil

    Claudio José Magon

  4. Brazilian Center of Research in Physics – CBPF/MCTI, Dr. Xavier Sigaud Street, 150, Urca, Rio de Janeiro, RJ, 22290-180, Brazil

    Cynthia Paola Contreras Medrano, Fred Jochen Litterst & Elisa Maria Baggio Saitovitch

  5. Institut für Physik Der Kondensierten Materie, Technische Universität Braunschweig, 38106, Braunschweig, Germany

    Fred Jochen Litterst

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Renda, C.G., Contreras Medrano, C.P., Costa, L.J.D. et al. Role of ferrocene-derived iron species in the catalytic graphitization of novolak resins. J Mater Sci 56, 1298–1311 (2021). https://doi.org/10.1007/s10853-020-05312-z

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