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Fluorinated poly(aryl ether)s (FPAEs) have attracted much attention due to their high thermal stability, excellent mechanical strength, and low dielectric constant. High‐molecular‐weight fluorinated poly(aryl ether) containing phenylethynyl (FPAE‐PE) is successfully synthesized by nucleophilic substitution between 3‐ethynylphenol and FPAE. The cross‐linked fluorinated poly(aryl ether) (C‐FPAE‐PE) is prepared by thermal treatment of FPAE‐PE at 300 °C. The thermal stability, dynamic thermomechanical property, and dielectric performance of C‐FPAE‐PE are systematically studied. C‐FPAE‐PE has excellent heat resistance with 5% weight loss temperature (Td5%) at 490 °C in air and high thermomechanical properties with storage modulus retention of 50% at 215 °C. C‐FPAE‐PE displays low and steady dielectric constant of 2.4 and dielectric loss of 0.004 at 215 °C, exhibiting potential applications in the field of microelectronics, communication technology, and energy storage as high‐temperature low dielectric materials.

The microstructures and macrostructures play a crucial role in the properties and applications of multifunctional materials. Herein, microscopic partition and macroscopic partition are combined by devising and preparing different modules that can be elaborately devised to possess specific performances. A two-dimensional (2D) 3-module Janus-type membrane multifunctionalized by conductive aeolotropism, magnetism and luminescence (defined as 3M-CML Janus-type membrane) is constructed via electro-spinning. The modular structure of 3M-CML Janus-type membrane is obtained by devising and constructing three different modules, including luminescence module (denoted as L module), conductive aeolotropism-luminescence module (marked as C-L module) and magnetism-luminescence module (named as M-L module). The results prove that almost no mutual detrimental influences exist among different modules owing to the macroscopic modular structure and Janus-type structure, which effectively avoids the negative interactions among different materials. Tb(BA)3phen/PVP nanofiber, [PMMA/Eu(BA)3phen]//[PMMA/PANI] Janus-type nanoribbon and [PMMA/Tb(BA)3phen]//[PMMA/Fe3O4] Janus-type nanoribbon are, respectively, selected as building units of the three modules, which further prevents the negative interactions among different materials and improves the versatility of 3M-CML Janus-type membrane. The luminescence, adjustable conductive aeolotropism and variable magnetism of 3M-CML Janus-type membrane are systematically discussed. Meanwhile, novel flexible four types of brand-new three-dimensional (3D) Janus-type tubes are obtained by rolling modularly devised 2D 3M-CML Janus-type membrane with different rolling schemes. As derivatives of the 2D 3M-CML Janus-type membranes, macroscopic 3D Janus-types tubes exhibit similar performances to 2D 3M-CML Janus-type membranes. The 2D Janus-type membrane and 3D Janus-type tube will have momentous applications in flexible electronics and nanodevices in the future.

A modularization design philosophy inspired by Rubik's Cube for the construction of multifunctional materials is proposed with 4M-EMF Janus film as a case study.