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The efficient synthesis of 2D polymers (2DPs) with tailorable structures and properties is highly desired but remains a considerable challenge. Here, the first solution synthesis of millimeter‐size crystalline covalent triazine frameworks (CTFs) with a clear lamellar structure, which can be exfoliated into micrometer‐size few‐layer 2DP sheets via both micromechanical cleavage and liquid sonication,...
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