Conducting polymers with conjugated backbones have been widely used in electrochemical energy storage, catalysts, gas sensors and biomedical devices. In particular, two-dimensional (2D) mesoporous conducting polymers combine the advantages of mesoporous structure and 2D nanosheet morphology with the inherent properties of conducting polymers, thus exhibiting improved electrochemical performance. Despite the use of bottom-up self-assembly approaches for the fabrication of a variety of mesoporous materials over the past decades, the synchronous control of the dimensionalities and mesoporous architectures for conducting polymer nanomaterials remains a challenge. Here, we detail a simple, general and robust route for the preparation of a series of 2D mesoporous conducting polymer nanosheets with adjustable pore size (5-20 nm) and thickness (13-45 nm) and controllable morphology and composition via solution-based self-assembly. The synthesis conditions and preparation procedures are detailed to ensure the reproducibility of the experiments. We describe the fabrication of over ten high-quality 2D-ordered mesoporous conducting polymers and sandwich-structured hybrids, with tunable thickness, porosity and large specific surface area, which can serve as potential candidates for high-performance electrode materials used in supercapacitors and alkali metal ion batteries, and so on. The preparation time of the 2D-ordered mesoporous conducting polymer is usually no more than 12 h. The subsequent supercapacitor testing takes ~24 h and the Na ion battery testing takes ~72 h. The procedure is suitable for users with expertise in physics, chemistry, materials and other related disciplines.
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