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. 2023 Jan 19;13(3):403.
doi: 10.3390/nano13030403.

Electrochemical Synthesis, Magnetic and Optical Characterisation of FePd Dense and Mesoporous Nanowires

Deepti Raj  1 , Gabriele Barrera  2 , Federico Scaglione  1 , Federica Celegato  2 , Matteo Cialone  1   3 , Marco Coïsson  2 , Paola Tiberto  2 , Jordi Sort  4   5 , Paola Rizzi  1 , Eva Pellicer  4
Affiliations

Electrochemical Synthesis, Magnetic and Optical Characterisation of FePd Dense and Mesoporous Nanowires

Deepti Raj et al. Nanomaterials (Basel). .

Abstract

Dense and mesoporous FePd nanowires (NWs) with 45 to 60 at.% Pd content were successfully fabricated by template- and micelle-assisted pulsed potentiostatic electrodeposition using nanoporous anodic alumina and polycarbonate templates of varying pore sizes. An FePd electrolyte was utilized for obtaining dense NWs while a block copolymer, P-123, was added to this electrolyte as the micelle-forming surfactant to produce mesoporous NWs. The structural and magnetic properties of the NWs were investigated by electron microscopy, X-ray diffraction, and vibrating sample magnetometry. The as-prepared NWs were single phase with a face-centered cubic structure exhibiting 3.1 µm to 7.1 µm of length. Mesoporous NWs revealed a core-shell structure where the porosity was only witnessed in the internal volume of the NW while the outer surface remained non-porous. Magnetic measurements revealed that the samples displayed a soft ferromagnetic behavior that depended on the shape anisotropy and the interwire dipolar interactions. The mesoporous core and dense shell structure of the NWs were seen to be slightly affecting the magnetic properties. Moreover, mesoporous NWs performed excellently as SERS substrates for the detection of 4,4'-bipyridine, showing a low detection limit of 10-12 M. The signal enhancement can be attributed to the mesoporous morphology as well as the close proximity of the embedded NWs being conducive to localized surface plasmon resonance.

Keywords: FePd; SERS; electrodeposition; mesoporous; nanowires.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
FESEM images of FePd NWs obtained by electrodeposition at Eon = −1.2 V on AAO membranes of (a,b) 20 nm and (c) 100 nm in diameter.
Figure 2
Figure 2
FESEM images of FePd NWs obtained by electrodeposition on PC membrane at Eon of (a) −1.05 V, (b) −1.15 V, (c) −1.2 V, and (d) −1.3 V.
Figure 3
Figure 3
Pulsed potentiostatic transients recorded during the deposition of FePd NWs on AAO templates of 20 and 100 nm in diameter, both for Eon = −1.2 V.
Figure 4
Figure 4
SEM images of Fe40Pd60 mesoporous NWs: (a) Porous-A, inset shows a single free NW at higher magnification; (b) magnified view of Porous-A; (c) Porous-B; (d) magnification of Porous-B; and insets of (b,d) give a closer look at the mesoporosity.
Figure 5
Figure 5
EDS maps of Porous-B NW (a) showing the presence and distribution of Pd (b) and Fe (c) throughout the length of the NW.
Figure 6
Figure 6
XRD pattern of the as-deposited Porous-A embedded in the AAO template.
Figure 7
Figure 7
Bright-field TEM images of Porous-A NWs: (a) A bunch of NWs, (b) diameter of a single NW and (c) close-up view of the wall.
Figure 8
Figure 8
Room-temperature hysteresis loops of (a) Dense-A and (b) Dense-B NW arrays by applying H along the direction parallel (PA) and perpendicular (PE) to the major axis of the NWs. Inset: enlargement of hysteresis loops at a low magnetic field.
Figure 9
Figure 9
Room-temperature hysteresis loops of (a) Porous-A sample and (b) Porous-B sample by applying H along the direction parallel (PA) and perpendicular (PE) to the major axis of the NWs. Inset: enlargement of hysteresis loops at a low magnetic field.
Figure 10
Figure 10
(a,b) SERS spectra shown by Porous-A NWs for bipy concentration of 10−10 M and 10−12 M respectively. (c,d) SERS spectra shown by nanoporous FePd thin film for bipy concentration of 10−6 M and 10−12 M respectively.
See this image and copyright information in PMC

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