In this study, we describe the preparation and characterization of a new class of thermoset hybrid networks containing aliphatic polyester and polyhedral oligomeric silsesquioxanes (POSS). The copper‐free 1,3‐dipolar cycloaddition click reaction of internal alkyne functionalized aliphatic polyester and multifunctional azido POSS with different concentrations led to highly crosslinked thermoset networks. The click reactions performed under ambient conditions (i.e., in tetrahydrofuran at room temperature for 1 day) in the absence of any catalyst. The chemical composition of hybrid networks and homogenous distribution of POSS molecules were confirmed by Fourier transform infrared spectroscopy and scanning electron microscopy with energy dispersive spectroscopy. The swelling ratios of hybrid networks were commonly decreased by increasing POSS‐N3 content and by changing polar solvents to apolar solvents. Thermogravimetric analysis results demonstrated that the thermal stability of hybrid networks increased with higher POSS feeding ratio. Tensile tests were applied to evaluate the mechanical properties of hybrid networks. Compared to neat aliphatic polyester, the mechanical properties of hybrid networks significantly improved. For instance, the tensile strength were enhanced from 5 MPa to 19 MPa by increasing the concentration of azido functionalized POSS from 10 to 40. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019, 57, 2222–2227

Synthesis of star‐shaped polystyrene (PS) and poly (methyl metachrylate) (PMMA) containing a polyhedral oligomeric silsesquioxane (POSS) core are fabricated by combination of atom transfer radical polymerization (ATRP) and copper (I) catalyzed azide‐alkyne cycloaddition (CuAAC) click reaction techniques. The synthetic route proceeds in two steps; firstly, clickable alkyne‐end functionalized polymeric arms and a POSS‐(N3)8 core are prepared independently by arm‐first approach using ATRP and nucleophilic substitution reaction of octa‐(3‐chloropropyl) silsesquioxane POSS‐(Cl)8 with sodium azide. Finally, the CuAAC click reactions between inorganic‐organic hybrid core POSS‐(N3)8 and alkyne functionalized PMMA and PS arms provide the targeted star‐shaped polymers. Their chemical structures and molecular characteristics are clearly confirmed by FT‐IR, 1H‐NMR, and GPC analyses. The obtained polymers are utilized as insulators for organic field effect transistors (OFETs) using perylene as an active n‐type organic semiconductor. Compared with linear PMMA and PMMA‐POSS, the POSS‐(PMMA)8 exhibited better output and transfer characteristics for the OFET device.

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