Improved graphitic carbon nitride (g‐C3N4) was synthesized through a unique one‐step cost‐effective technique involving a dynamic gas bubbling phenomenon using ammonium chloride (NH4Cl) as a bubbling agent. An extensive investigation was carried out to optimize the weight ratio of NH4Cl and melamine during the thermal pyrolysis process. Here, we report an improved form of g‐C3N4 namely “expanded g‐C3N4” with increased interlayer distance and remarkable volume expansion. The surface area of this improved version has notably increased leading to higher photocatalytic efficiency as compared with its counterpart, an synthesized without adding NH4Cl. Synthesized photocatalyst materials were further used to study the Rhodamine B photodegradation under visible light. It was observed that the expanded g‐C3N4 showed a 2.4 times higher photodegradation rate than its counterpart and degraded 94% of the dye in just 30 min.
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