Synthesis of Fe-Fe2B catalysts via solvothermal route for hydrogen generation by hydrolysis of NaBH4

Year 2018, Volume: 3 Issue: 1, 51 - 62, 26.03.2018

Mustafa Barış , Tuncay Şimşek Hatice Taşkaya Arun K. Chattopadhyay

https://doi.org/10.30728/boron.348291

Cited By: 5

Abstract

In this study, iron sulfate
heptahydrate (FeSO_4.7H₂O) and sodium borohydride (NaBH₄)
were used to synthesize Fe-Fe₂B nanocrystals
via the solvothermal route. Synthesis of Fe-Fe₂B nanocrystals was
carried out under Argon (Ar) gas atmosphere with aqueous solutions of FeSO₄.7H₂O
and NaBH₄ at various concentrations and reaction time. The phases
and microstructures of nanocrystals thus formed were characterized by X-Ray
diffraction (XRD) spectroscopy and scanning electron microscopy (SEM). Surface
areas of nanocrystals were measured by a surface area and pore-size analyzer using
nitrogen adsorption-desorption method together with Brunauer-Emmett-Teller
(BET) equation. The vacuum dried nanoparticles were calcined under both Ar and
air at 500 ºC. Nano-cylindrical structures Fe-Fe₂B were observed
while calcinating under Ar atmosphere; whereas more irregular shaped particles
were obtained by calcination under air. The surface areas of nanocylinders were
determined as 12 m²/g, 5.5 m²/g and 16.5 m²/g,
for vacuum dried, Ar-calcined and O₂-calcined products respectively.
The catalytic effect of those nanocrystals for hydrogen generation were studied
by determining reaction rates in aqueous alkaline solutions of NaBH₄.
Their catalytic activities were investigated by varying the amount of
catalysts, and the concentrations of NaBH₄ and NaOH. The effect of
temperature on the catalytic activity was also studied by varying the temperatures
from 25-70 °C. It was noticed that the catalytic activity of vacuum dried
nanocrystals was the highest, and it decreased with the increase in NaOH
concentration. With 0.01 g of Fe-Fe₂B
catalyst in 1 % w/w NaBH₄ concentration at 25 °C, the hydrogen
production rate was 570 mL of H₂.g^-1.m^-1,
which reached to 1230 at 50 °C and
2700 mL at 70 °C. 

Keywords

Fe2B, nanocrystal, solvothermal method, hydrogen production

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