Surface
activation of catalysts is known to be an efficient process to enhance
their activity in catalytic processes. The activation process includes
the generation of oxygen vacancies, changing the nature of the catalyst
surface from acidic to basic and vice versa, and the reduction of
catalyst surface by H
2
. On the other hand, magnetically
separable catalysts are highly beneficial for their utilization in
water or biological fluid-based catalytic processes, as they can be
easily guided to the target site and recovered. Here, we present the
fabrication of CoFe
2
O
4
and composites of Co
3
O
4
/CoFe
2
O
4
/α-Fe
2
O
3
and Co/CoFe
2
O
4
/α-Fe
2
O
3
through solution combustion process to utilize
them as catalysts for 4-nitrophenol (4-NP) reduction. Although none
of the as-prepared CoFe
2
O
4
and Co
3
O
4
/CoFe
2
O
4
was seen to be active
in 4-NP reduction reaction, the surface of the composite gets activated
by borohydride (NaBH
4
) treatment to act as a highly active
catalyst for 4-NP reduction. X-ray photoelectron spectroscopy of the
composite revealed the formation of metal-hydroxide (M–O–H)
species of both Co and Fe at its surface due to borohydride treatment.
The mechanism of the surface activation and the dynamics of 4-NP reduction
of the surface-activated composite have been studied, proposing a
possible pathway for the reduction of 4-NP.