Nanocatalyst materials
based on metal nanoparticles (NPs) deposited
on mesoporous carbon substrates are widely used in catalysis and energy
storage; however, conventional wet-chemical deposition methods based
on the reduction of metal salts are not always the best choice when
looking for a process ensuring easy scalability and low environmental
impact. Moreover, additional surface functionalization steps, such
as the addition of nitrogen- or oxygen-containing groups, are more
and more explored to increase the activity or the chemical stability
of catalysts. In this work, we investigate a new methodology for the
fabrication of nickel/carbon nanocatalysts relying on a low-pressure
radio frequency plasma treatment of solid (powder) precursors. A mesoporous
carbon xerogel is used as support for nickel NPs synthesized through
the decomposition of an organometallic nickel precursor in a plasma
discharge. Different plasma treatment conditions and chemical environments
are applied by varying the plasma power and the gas mixture injected
into the plasma chamber (Ar, N2, NH3, and O2). The nucleation kinetics of nickel NPs, their morphology
evolution, and chemical state were fully characterized by combining
analytical techniques such as in situ optical emission spectroscopy,
transmission electron microscopy, X-ray diffraction, and X-ray photoelectron
spectroscopy. Results indicate that the plasma chemistry and conditions
strongly influence the organometallic compound decomposition as well
as the size and the oxidation state of the homogeneously dispersed
nickel NPs. We compare the organometallic precursor degradation efficiency
for each plasma by defining a rational “activation power”
associated with each plasma chemistry. Moreover, simultaneous carbon
substrate functionalization is obtained through plasma treatment,
which demonstrates the high versatility of the plasma fabrication
for developing green and efficient catalysts and energy materials.