Scalable Preparation of High‐Quality Microwave‐Assisted Reduced Graphene Oxide via Spatial Configuration Engineering

Abstract The non‐uniform heating phenomenon in microwave‐assisted synthesis of carbon materials has persistently posed a core challenge restricting the realization of industrial‐scale applications for microwave technology. Here, an innovative microwave reduction strategy based on spatial configuration engineering is proposed, solving the problem of uneven product quality in the scale‐up preparation of microwave‐assisted reduced graphene oxide (m‐rGO). The corona‐discharge‐free and fully exposed irradiation areas jointly determine the stability of batch reduction and quality of m‐rGO. The quality of the m‐rGO is significantly improved by preferential optimization of the process parameters, achieving an I D / I G ratio as low as 0.12 and an excellent electrical conductivity of 13486 S m −1 , with a yield of ≈70 g per batch. Due to its high conductivity, lightweight, graphene‐based materials have emerged as promising candidates in absorption‐dominated electromagnetic interference (EMI) shielding fields. A microwave‐assisted reduced graphene oxide/polyurethane (m‐rGO/PU) film is prepared with a thickness of 90 µm, exhibiting outstanding EMI SE of up to 40 dB in the X‐band. This study provides a strategy for mitigating the quality variability associated with microwave heating technology in the scale‐up preparation of various advanced carbon materials, facilitating the industrial application of microwave technology.