Efficient nanostructured heterogeneous catalysts by electrochemical etching of partially crystallized Fe-based metallic glass ribbons

doi:10.1016/j.jmst.2020.06.016

Abstract

Abstract:

Although an increasing interest has been attracted to further develop heterostructured catalysts from metallic glasses (MGs) by heat treatment, overcoming surface oxidation effect is still a critical problem for such environmental catalysts. Herein, a short-time electrochemical etching of partially crystallized Fe-based ribbons in 0.3 M H₃PO₄ electrolyte enables the formation of honeycomb-like nanoporous structure as effective catalytic active sites in Fenton-like process. Studies of structure and surface morphologies reveal that the formation of nanoporous structure by potentiostatic etching originates from electrochemical potential difference of nanocrystals (α-Fe (Si) and Fe₂B) and residual amorphous phase in partially crystallized ribbons, where Fe₂B having a lower open circuit potential tends to be selectively dissolved. Simultaneously, thin oxide layer after electrochemical etching exposes more active sites for H₂O₂ activation and provides an effective protection of nanocrystals from massive loss during etching. Investigation of optimal processing conditions suggests that the selection of electrolyte plays an important role; dye degradation rates of etched ribbons in HNO₃ and Na₂SO₄ electrolytes can also achieve at least 2 times higher than that of as-annealed ribbons. This work holds the promise to develop novel environmental catalysts by effective electrochemical etching of partially crystallized ribbons.

Key words: Metallic glass, Nanoporous structure, Crystallization, Electrochemical etching, Selective dissolution

Qiaoyue Zhang, Shun-Xing Liang, Zhe Jia, Wenchang Zhang, Weimin Wang, Lai-Chang Zhang. Efficient nanostructured heterogeneous catalysts by electrochemical etching of partially crystallized Fe-based metallic glass ribbons[J]. J. Mater. Sci. Technol., 2021, 61: 159-168.

Figures/Tables 12

Fig. 1. XRD patterns of as-annealed FeSiB-A520, FeSiB-A560 and FeSiB-A600 ribbons.

Fig. 2. High resolution (a) Fe 2p and (b) O 1s spectra of as-annealed FeSiB-A520, FeSiB-A560 and FeSiB-A600 ribbons.

Fig. 3. (a) Potentiodynamic polarization curves and (b) electrochemical impedance spectroscopy of as-annealed FeSiB-A520, FeSiB-A560 and FeSiB-A600 ribbons.

Fig. 4. BR3B-A dye decolorization by electrochemical-etched (a) FeSiB-A520, (b) FeSiB-A560 and (c) FeSiB-A600 varying from 0 s to 720 s in 0.3 M H3PO4 solution. Quenching effect by 0.01 - 1.0 M TBA on 180s-etched (d) FeSiB-A520, (e) FeSiB-A560 and (f) FeSiB-A600.

Fig. 5. UV-vis spectra of BR3B-A dye decolorization by: (a) as-annealed and (b) 180s-etched FeSiB-A520; (c) as-annealed and (d) 180s-etched FeSiB-A560; (e) as-annealed and (f) 180s-etched FeSiB-A600.

Fig. 6. XRD patterns of FeSiB-A520 after electrochemical etching from 0 s to 720 s in 0.3 M H3PO4.

Fig. 7. Surface morphologies of FeSiB-A520 electrochemically etched at (a) 90, (b) 180 s and (c) 720 s before BR3B-A dye degradation, which are correspondingly denoted as: xxx (etching time) - Be. (d) (e) (f) surface morphologies of (a) (b) (c) after dye degradation, which are correspondingly denoted as: xxx (etching time) - Af.

Fig. 8. (a) Reusability of FeSiB-A520 and (b) corresponding decolorization rate after stabilization. (c) and (d) Surface morphologies of 9th-reused FeSiB-A520 ribbons.

Fig. 9. Reaction rate constants kobs of partially crystallized ribbons (FeSiB-A520, FeSiB-A560 and FeSiB-A600) 180s-etched in (a) 0.05 - 1.0 M H3PO4 solution, (b) HNO3, H3PO4, H2SO4 and HCl solution (with equivalent H+) and (c) NaNO3, Na3PO4, Na2SO4 and NaCl solution (with equivalent anion at pH 6.0).

Fig. 10. Surface morphologies of 180s-etched FeSiB-A520 in (a) (b) 0.9 M HCl, (c) (d) 0.5 M H2SO4 and (e) (f) 0.9 M HNO3 solution before and after dye degradation. Surface morphologies before and after dye degradation are denoted as: xxx (acid) - Be and xxx (acid) - Af, respectively.

Fig. 11. Surface morphologies of 180s-etched FeSiB-A520 in (a) NaCl, (b) Na3PO4, (c) Na2SO4 and (d) NaNO3 solution at pH 6.0. The concentrations of all electrolytes are 0.3 M.

Fig. 12. Schematic illustration of H2O2 activation process by partially crystallized Fe78Si9B13 ribbons with electrochemical etching.

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