Herein, we report on the evolution of superparamagnetic
behavior
of Nb–Cr–Ta–V–W refractory high entropy
alloy (RHEA) nanoparticles synthesized by a facile mechanical pulverization
(high-energy ball milling) technique. Detailed X-ray diffraction (XRD),
scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy
(EDS) analyses have been made to evaluate the structure, morphology,
compositional, and elemental distribution characteristics of RHEA
nanoparticles and further compared with the bulk. XRD and SEM data
coupled with EDS analyses indicate that the nano-RHEA retains the
parent crystal structure and phase, but the size dramatically decreases
with milling time. The average crystallite size decreases from ∼32
to ∼12 nm with an increasing milling time to 16 h. While the
bulk samples exhibit diamagnetic behavior, interestingly, RHEA nanoparticles
demonstrate superparamagnetic nature. Magnetic measurements, in both
room temperature and cryogenic conditions, provide evidence of the
temperature-independent superparamagnetic nature of the RHEA nanoparticles.
Furthermore, the saturation magnetization value exponentially increased
with milling time and stabilized after 8 h of pulverization, whereas
the magnetic domain size followed an opposite trend. We believe drastic
reduction in the magnetic domain size is responsible for this unusual
and unexpected superparamagnetic pattern of the RHEA nanoparticle,
which opens up a new route for low-cost magnetic applications under
harsh environment conditions.