Skip to main content
SpringerLink
Log in

Oxide nanolayer formation on surface of modified blast furnace sludge particles during voltammetric cycling in alkaline media

  • Original Paper
  • Published:
Journal of Solid State Electrochemistry Aims and scope Submit manuscript

Abstract

Knowledge of the properties of metallurgical waste is essential for the assessment of their recycling. In this work, the formation of iron oxide nanolayers during voltammetric cycling in 1 M NaOH on the particle surface of blast furnace sludge after acid leaching (BFSL) was studied. Most importantly, the effect of hydrogen on these processes was of particular interest. For these purposes, the study combines electrochemical methods, cyclic voltammetry on solid and carbon paste electrodes, with analytical optical methods (TEM). On the solid iron electrode surface as a model system, nanostructured magnetite (Fe3O4) was identified as the main oxidation product, and, to a lesser extent, also maghemite (γ-Fe203). It was found that the charges corresponding to Fe3O4 formation and its reduction together with the hydrogen evolution reaction (HER) occurring at E = − 1500 mV depend on the number of cycles and have a similar course. Additionally, in the first phase of the cycling, the accumulation of maghemite on the solid Fe-electrode surface during cycling affects the growth of the oxide layer and catalytically increases the yield of the HER. Concerning the measurement with BFSL-modified CPE, on the BFSL surface, haematite is transformed into magnetite during cycling, resulting in the same Fe3O4 nanolayer as on the solid iron electrode. In this layer, the same redox processes take place, including the influence of hydrogen in the initial stage of cycling.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4
Fig. 5
Fig. 6
Fig. 7
Fig. 8
Fig. 9

Similar content being viewed by others

References

  1. Das B, Prakash S, Reddy PSR, Misra VN (2007) An overview of utilization of slag and sludge from steel industries. Resour Conserv Recycl 50(1):40–57

    Article  Google Scholar 

  2. Huang X, Zhao H, Li X, Qiu W, Wu W (2007) Performance of planar SOFCs with doped strontium titanate as anode materials. Fuel Cell Bull 7:12–16

    Article  Google Scholar 

  3. Langová Š, Leško J, Matýsek D (2009) Selective leaching of zinc from zinc ferrite with hydrochloric acid. Hydrometallurgy 95(3-4):179–182

    Article  Google Scholar 

  4. Asadi ZB, Mowla D, Shariat MH, Fathi KJ (1997) Zinc recovery from blast furnace flue dust. Hydrometallurgy 47(1):113–125

    Article  Google Scholar 

  5. Steer JM, Griffiths AJ (2013) Investigation of carboxylic acids and non-aqueous solvents for the selective leaching of zinc from blast furnace dust slurry. Hydrometallurgy 140:34–41

    Article  CAS  Google Scholar 

  6. Volpi E, Olietti A, Stefanoni M, Trasatti SP (2015) Electrochemical characterization of mild steel in alkaline solutions simulating concrete environment. J Electroanal Chem 736:38–46

    Article  CAS  Google Scholar 

  7. Hugot-Le Goff A, Flis J, Boucherit N, Joiret S, Wilinski J (1990) Use of Raman spectroscopy and rotating split ring disk electrode for identification of surface layers on iron in 1M NaOH. J Electrochem Soc 137:2684–2690

    Article  CAS  Google Scholar 

  8. Joiret S, Keddam M, Nóvoa X, Pérez M, Rangel C, Takenouti H (2002) Use of EIS, ring-disk electrode, EQCM and Raman spectroscopy to study the film of oxides formed on iron in 1M NaOH. Cem Concr Compos 24(1):7–15

    Article  CAS  Google Scholar 

  9. Nieuwoudt MK, Comins JD, Cukrowski I (2011) The growth of the passive film on iron in 0.05 M NaOH studied in situ by Raman micro-spectroscopy and electrochemical polarisation. Part I: near-resonance enhancement of the Raman spectra of iron oxide and oxyhydroxide compounds. J Raman Spectrosc 42(6):1335–1339

    Article  CAS  Google Scholar 

  10. Nieuwoudt MK, Comins JD, Cukrowski I (2011) The growth of the passive film on iron in 0.05 M NaOH studied in situ by Raman microspectroscopy and electrochemical polarization. Part II: in situ Raman spectra of the passive film surface during growth by electrochemical polarization. J Raman Spectrosc 42(6):1353–1365

    Article  CAS  Google Scholar 

  11. Flis-Kabulska I, Zakroczymski T, Flis J (2007) Accelerated entry of hydrogen into iron from NaOH solutions at low cathodic and low anodic polarisations. Electrochim Acta 52(9):2966–2977

    Article  CAS  Google Scholar 

  12. Song I, Gervasio D, Payer JH (1996) Electrochemical behaviour of iron and iron oxide thin films in alkaline (1 M KOH) aqueous solution: a voltammetry study for cathodic instability of coating/metal interface. J Appl Electrochem 26:1045–1052

    Article  CAS  Google Scholar 

  13. Doyle RL, Lyons MEG (2013) An electrochemical impedance study of the oxygen evolution reaction at hydrous iron oxide in base. Phys Chem Chem Phys 15(14):5224–5237

    Article  CAS  PubMed  Google Scholar 

  14. Švancara I, Kalcher K, Walcarius A, Vytřas K (2012) Electroanalysis with carbon paste electrodes, 1st edn. CRC Press, Boca Raton

    Book  Google Scholar 

  15. Akhtar A, Ghaffarinejad A, Hosseini SM, Manteghi F, Maminejad N (2015) Electrocatalytic hydrogen production by bulk and nano Fe2O3 and carbon nanotube modified with Fe2O3. J Electroanal Chem 739:73–83

    Article  CAS  Google Scholar 

  16. Fetisov VB, Ermanov AN, Belysheva GM, Fetisov AV, Kamyshov VM, Brainina KZ (2004) Electrochemical dissolution of magnetite in acid solutions. J Solid State Electrochem 8:565–571

    Article  CAS  Google Scholar 

  17. Grygar T (1997) Dissolution of pure and substituted goethites controlled by the surface reaction under conditions of abrasive stripping voltammetry. J Solid State Electrochem 1(1):77–82

    Article  CAS  Google Scholar 

  18. Grygar T (1998) Phenomenological kinetics of irreversible electrochemical dissolution of meta-oxide microparticles. J Solid State Electrochem 2(3):127–136

    Article  CAS  Google Scholar 

  19. Mutombo P, Hackerman N (1997) Potential decay behavior of iron in dilute nitric acid. J Solid State Electrochem 1(3):194–198

    Article  CAS  Google Scholar 

  20. Novák V, Raška P, Matýsek D, Kostura B (2018) Electrochemical characterization of fine-grained blast furnace sludge after acid leaching using carbon paste electrode. J Solid State Electr 22(11):3457–3466

    Article  Google Scholar 

  21. Liu M, Cheng X, Zhao G, Li X, Pan Y (2016) Corrosion resistances of passive films on low-Cr steel and carbon steel in simulated concrete pore solution. Surf Interface Anal 48(9):981–989

    Article  CAS  Google Scholar 

  22. Freire L, Catarino MA, Godinho MI, Ferreira MJ, Ferreira MGS, Simoes AMP, Montemor MF (2012) Electrochemical and analytical investigation of passive films formed on stainless steels in alkaline media. Cement Concrete Comp 34(9):1075–1081

    Article  CAS  Google Scholar 

  23. Allanore A, Lavelaine H, Valentin G, Birat JP, Delcroix P, Lapicque F (2010) Observation and modeling of the reduction of hematite particles to metal in alkaline solution by electrolysis. Electrochim Acta 55(12):4007–4013

    Article  CAS  Google Scholar 

  24. Monteiro JF, Ivanova YA, Kovalevsky AV, Ivanou DK, Frade JR (2016) Reduction of magnetite to metallic iron in strong alkaline medium. Electrochim Acta 193:284–292

    Article  CAS  Google Scholar 

  25. Das NK, Shoji T (2013) An atomic study of hydrogen effect on the early stage oxidation of transition metal surfaces. Int J Hydrogen Energ 38(3):1644–1656

    Article  CAS  Google Scholar 

  26. Schmuki P, Büchler M, Virtanen S, Isaacs HS, Ryan MP, Böhni H (1999) Passivity of Iron in alkaline solutions studied by in situ XANES and a laser reflection technique. J Electrochem Soc 146:2097–2102

    Article  CAS  Google Scholar 

  27. Davodi F, Mühlhausen E, Tavakkoli M, Sainio J, Jiang H, Gökce B, Marzun G, Kallio T (2018) Catalyst support effect on the activity and durability of magnetic nanoparticles: toward design of advanced electrocatalyst for full water splitting. ACS Appl Mater Interfaces 10(37):31300–31311

    Article  CAS  PubMed  PubMed Central  Google Scholar 

  28. Weinrich H, Gehring M, Tempel H, Kungl H, Eichel RA (2019) Electrode thickness-dependent formation of porous iron electrodes for secondary alkaline iron-air batteries. Electrochim Acta 314:61–71

    Article  CAS  Google Scholar 

  29. Shibli SMA, Sebeelamol JN (2013) Development of Fe2O3–TiO2 mixed oxide incorporated Ni–P coating for electrocatalytic hydrogen evolution reaction. Int J Hydrog Energy 38(5):2271–2282

    Article  CAS  Google Scholar 

  30. Zou X, Gu S, Cheng H, Lu X, Zhou Z, Li C, Ding W (2015) Facile electrodeposition of iron films from NaFeO2 and Fe2O3 in alkaline solutions. J Electrochem Soc 162(1):D49–D55

    Article  CAS  Google Scholar 

Download references

Funding

This paper was created within the frame of the project number SP2019/142 financed by the Ministry of Education, Youth and Sports of the Czech Republic and the project number CZ.02.1.01/0.0/0.0/17_049/0008426 financed by Operational Programme Research, Development and Education under the auspices of the Ministry of Education, Youth and Sports of the Czech Republic.

Author information

Authors and Affiliations

  1. Department of Chemistry, VŠB - Technical University of Ostrava, 17. listopadu 2172/15, 708 00, Ostrava-Poruba, Czech Republic

    V. Novák, B. Kostura, P. Raška & J. Leško

  2. Centre for Advanced Innovation Technologies, VŠB-Technical University of Ostrava, 17. listopadu 2172/15, 708 00, Ostrava-Poruba, Czech Republic

    K. Peterek Dědková

  3. Leibniz Institute for Solid State and Materials Research Dresden, Helmholtzstraße 20, 01069, Dresden, Germany

    R.G. Mendes & T. Gemming

Authors
  1. V. Novák
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. B. Kostura
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. P. Raška
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. K. Peterek Dědková
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. R.G. Mendes
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. T. Gemming
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. J. Leško
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to B. Kostura.

Ethics declarations

Competing interests

The authors declare that they have no conflicts of interest.

Additional information

Publisher’s note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Novák, V., Kostura, B., Raška, P. et al. Oxide nanolayer formation on surface of modified blast furnace sludge particles during voltammetric cycling in alkaline media. J Solid State Electrochem 25, 365–372 (2021). https://doi.org/10.1007/s10008-020-04819-4

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s10008-020-04819-4

Keywords

Search

Navigation