Details

Autor(en) / Beteiligte

• do Nascimento, Renata Flávia Ferraz
• Ferreira, Aldebarã Fausto
• da Costa Carvalho, Gabriela
• de Lemos Campello, Sergio
• Rodrigues, Alexandre Ricalde
• de Azevedo, Walter Mendes

Titel

α-Fe@MIL-100(Fe) composites obtained by one-pot sonochemical synthesis

Ist Teil von

• Journal of nanoparticle research : an interdisciplinary forum for nanoscale science and technology, 2024-03, Vol.26 (3), p.59

Ort / Verlag

Dordrecht: Springer Netherlands

Erscheinungsjahr

2024

Link zum Volltext

Quelle

SpringerLink

Beschreibungen/Notizen

• In this work, we present a one-pot synthesis route to prepare a new composite materials of iron (α-Fe) and a metal–organic framework (MOF) of iron, the MIL-100(Fe), using the sonochemical process. The experimental setup consists of applying high-power ultrasonic pulses to a water-dimethylformamide (H 2 O-DMF) (1:1) solution containing iron powder, 1,3,5-benzenetricarboxylic acid (H 3 BTC), and nitrate (NO 3− ). X-ray diffractions and the FT-IR measurements confirm that MIL-100(Fe) was obtained and the difference parameter Δ between the asymmetric and symmetric infrared mode of the order of 250 cm −1 is an indication that the carboxyl oxygen is coordinated through an unidentate interaction with iron Fe(III) in the MOF structure, also the presence of α-iron(Fe 0 ) in the composite was confirmed by the appearance of the diffraction peak at 44.7°. Scanning electron microscopy showed a rod-like morphology for the MIL-100(Fe) and the magnetization measurements suggest a ferromagnetic behavior with maximum magnetization ( M S ) varying as a function of synthesis parameter Fe 0 , H 3 BTC, and nitrate ratio. Higher and lower M S , of 12.52 emu.g −1 and 0.34 emu.g −1 , were obtained for Fe 0 :H 3 BTC:HNO 3 ratio of 3:1:3.5 and 1:1:3.5, respectively. The largest and smallest Brunauer–Emmett–Teller surface areas of 1490.2 m 2 .g −1 and 666.4 m 2 .g −1 were obtained for the Fe 0 :H 3 BTC:HNO 3 ratio of 1:1:3.5 and Fe 0 :H 3 BTC:NaNO 3 of 1:1:20, respectively. Decomposition of nitrate anion, NO 3 - and DMF, under ultrasound producing perhydroxyl radicals, HO 2 •, and hydrogen peroxide (H 2 O 2 ) and hydrogen (H 2 ) has been used to explain the mechanism for the α-Fe@MOF-100(Fe) magnetic composites preparation. Graphical Abstract