Resolving Triblock Terpolymer Morphologies by Vapor-Phase Infiltration

Abstract

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Selective sequential infiltration synthesis of ZnO in the liquid crystalline phase of silicon-containing rod-coil block copolymers

“…ZnO selectively infiltrates the PMPCS microdomains with high fidelity, which enhances the contrast between the PS and PMPCS and reveals the core-shell nanostructures of the DSM terpolymer. Compared with ZnO infiltration into the crystalline PLA microdomains of PDMSB-b-PS-b-PLA in our previous work, 30 the ZnO infiltration in this work demonstrated much improved uniformity and selectivity within the liquid crystalline PMPCS microdomains, and cylindrical as well as coreshell cylindrical and perforated lamellar ZnO/BCP composites were produced.…”

“…5 We previously used SIS to selectively deposit ZnO into one organic microdomain (PLA) of a silicon-containing triblock terpolymer, PDMSB-b-PS-b-PLA where PS represents polystyrene, producing three-dimensional (3D) organic/metal oxide/SiO x composites after etching, and helping to resolve the 3D morphology of lamellar and perforated lamellar morphologies. 30 However, the ZnO formed nanoparticles within the PLA rather than a uniform distribution and ZnO was also present in the PDMSB, attributed to prior atmospheric oxidation of the Si in that block. There have not been other investigations combining SIS with a Si-containing BCP.…”

Recent Advances in Sequential Infiltration Synthesis (SIS) of Block Copolymers (BCPs)

“…These are by far the most commonly utilized techniques for the dimensional characterization of nanomaterials, requiring simple calibration of the magnification using calibration samples with features in the same dimensional range as the analyzed ones [ 57 ]. Electron microscopy has been widely reported for the morphological characterization of block copolymers nanopatterns or polymeric films treated with SIS of inorganic compounds [ 31 , 35 , 51 , 56 , 58 , 59 , 60 , 61 ]. Electron microscopy is often complemented by energy-dispersive X-ray (EDX) spectroscopy.…”

“…It is based on the detection of characteristic X-rays produced from the interaction of high-energy electrons with the specimen atoms, allowing the univocal analysis of the elemental composition. This technique has been used for both in-plane and in-depth chemical characterization of the infiltrated polymer [ 31 , 43 , 51 , 59 , 61 , 62 , 63 ].…”

“…In the same manuscript the authors also report a cross-sectional 3D reconstruction of the heterostructures, obtained by EDX-STEM tomography. Recently, HAAFD-STEM imaging was used to resolve the infiltrated ZnO at the junction of vertical and horizontal PLA in a three-dimensional structure of poly(1,1-dimethyl silacyclobutane- b -styrene- b -lactide) (PDMSB- b -PS- b -PLA) triblock terpolymer with PS and PLA blocks domains [ 61 ].…”