Abstract

In this chapter, we study the kinetics and thermodynamics of a 35 kg mol\(^{-1}\) gyroid-forming polystyrene-b-polyisoprene-b-poly(ethylene oxide) (ISO) linear triblock terpolymer during solvent vapour annealing (SVA) using grazing-incidence small-angle X-ray scattering (GISAXS). GISAXS is the most direct means by which to study the microphase-separated morphology of a block copolymer in situ during SVA, allowing simultaneous characterisation of both in- and out-of-plane electron density correlations in the film over a macroscopically large area in real time. We anneal the terpolymer films in various solvent vapours (chloroform, tetrahydrofuran, and methanol) and their mixed vapours (tetrahydrofuran and methanol) and identify the resulting microphase-separated morphologies and long-range order upon varying the maximum solvent concentration and removal rate. The results provide crucial information regarding the behaviour of gyroid-forming triblock terpolymer thin films when exposed to solvent vapour, and therefore constitute a first step towards rational design of SVA protocols to successfully and reliably achieve large domains of the alternating gyroid morphology for optical metamaterial applications.

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