Semiconductor-based photocatalytic and photoelectrochemical
water
splitting is an ultimate source of hydrogen generation for tackling
the ongoing fuel crisis. In this context, we have synthesized a highly
porous N-rich g-C3N4 metal-free, nontoxic semiconductor
through the polycondensation method. In the present work, we have
discussed the major changes in the morphology of g-C3N4 after acidic exfoliation thoroughly by using transmission
electron microscopy (TEM) and scanning electron microscopy (SEM) studies.
The chemical purity of the as-synthesized materials was analyzed by
using powder X-ray diffraction (PXRD). The specific surface area and
porosity of the materials were obtained through Brunner–Emmet–Teller
(BET) surface area studies. Besides this, the electronic structure
of g-C3N4 was discussed through X-ray absorption
near-edge spectroscopy (XANES), and the elemental composition was
determined by using X-ray photoelectron spectroscopy (XPS). Moreover,
the dependency of the sacrificial agents of g-C3N4 was discussed in detail by using sodium sulfide/sodium sulfite (Na2S/Na2SO3) and triethanolamine (TEOA).
It was observed that exfoliated g-C3N4 shows
remarkable hydrogen evolution in the presence of TEOA and an efficient
quantum yield up to 12%, which is 1.7-fold higher than in the presence
of Na2S/Na2SO3 (7%). Furthermore,
to harness most of the solar light spectrum, a high current density
and improved Faradaic efficiency during the photoelectrocatalysis
have been reported.