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Membranes 2014, 4 294 ρ=1 The nominal volume fraction of the filler, φdN , is described as: φN = Vd add 1−wd +wd (1) ρc ρd where wd is the weight fraction of the dispersed phase (IL or ETS-10) in the continuous matrix, ρd and ρc are the densities of the dispersed and the polymer phase in the continuous matrix in Table 1. d V +V (2) cd where Vd and Vc are the ideal contributions of the dispersed and continuous phases, the inorganic filler and organic continuous matrix, respectively, to the total volume, defined as the mass of the organic and inorganic components added to the composite, divided by the pure polymer or filler density. In this work, the CS polymer or IL/CS hybrid are considered as continuous matrix for the 2- and 3-component MMMs, respectively. The measured density values are always smaller than the theoretical values. This accounts for the void fraction created in the MMM upon addition of the porous ETS-10 nanoparticles, which resulted in lower density. This is the reason why the ideal MMM morphology, where a perfect adhesion between the organic and the inorganic phase, as depicted in Figure 1a, is seldom present in reality and the non-ideal free-volume in Figure 1b, attributed to poor interfacial contact between dispersed and continuous phases (Figure 1c), must be taken into account. The true filler volume fraction, φd, was calculated by comparing the experimental and the theoretical densities, when the void volume fraction can be calculated as [35]: φ =φN(1−φ) ddv (3) φv =1− ρm (4) ρadd The void fraction increased significantly for the two-component ETS-10/CS and the three-component ETS-10/IL/CS MMMs above that of CS membranes. This increase can be attributed to several factors: polymer crystallinity, interphase voids between the particles and the porosity of the crystals themselves [35,36]. The highest value of the density for the IL/CS membrane and the negative value for the void volume fraction may be attributed to the intimate contact between IL and CS. Table 4 summarises the solubility values calculated from thermo gravimetrical sorption experiments. It is worth noticing that the solubility values of the single components do not agree with the additive rule, which correlates with the observation of non-idealities and void fraction calculations in Table 3, in agreement with the MMM morphologies in Figure 1. The CO2 solubility increases upon addition of ETS-10 particles, which agrees with our assumption that the incorporation of this alkaline titanosilicate favours CO2 permeation due to its adsorption affinity toward CO2. The N2 solubility decreased about 42% in ETS-10/CS MMMs, which was attributed to the molecular sieve effect of the nanoporous titanosilicate. The average pore opening of ETS-10 is 0.8 nm [37]. The N2 solubility in the three-component ETS-10/IL/CS MMMs was further reduced, due to the incorporation of the highlyPDF Image | Synthesis and Characterisation of ETS-10 Acetate-based Ionic
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