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Chapter 4 Nafion®/H-ZSM-5 composite membranes with superior performance for DMFCs 2. Experimental 2.1. Materials DE2020 Nafion® dispersion (20wt. % Nafion® + 80wt. % water and VOCs, 1000 equivalent weight (EW)) was purchased from Ion Power Inc. (U.S.A.). DMSO was purchased from Aldrich (Germany). E-TEK electrodes were purchased from E-TEK DeNora (U.S.A.). Aluminum sulfate hexadecanohydrate (Al2(SO4)3*16H2O, 98%) and tetraethylorthosilicate (TEOS, 98%) was purchased from Aldrich. Tetrapropylammonium hydroxide (TPAOH, 20% aqueous solution) was purchased from Sigma. 2.2. Seeds synthesis Polymer-zeolite composite membranes can be prepared using small zeolite crystals obtained by milling of big crystals. A precise control of the process parameters is needed for controlling crystal size and homogeneity. Besides, nanosized zeolite crystals can be prepared by hydrothermal synthesis, although long ageing times and/or durations are generally required for obtaining small and uniform crystal sizes by conventional heating methods [19, 20]. Microwaves-assisted heating is an attractive strategy for reducing synthesis time and obtaining uniform nanocrystals [21]. In the present study microwave heating is used to prepare ZSM-5 nanosized crystals within a few hours, starting from sol with a Si/Al molar ratio in the range 25-100. Mother sols were prepared by mixing TEOS (98%), ultrapure water (18.2 MΏ) and TPAOH (20% aqueous solution). Al2(SO4)3*16H2O (98%) was used as Al precursor. The mother sol composition was: xAl2O3 :1SiO2 : 0.4TPAOH : 19.5H2O : 4C2H5OH. The alumina concentration x was varied in the range 0.05-0.2 (Si/Al=25-100) in the mother sol. Sols were aged at room temperature (25°C) under stirring for 24 h in air. A sol quantity of about 20 g was used for each experiment. The microwave assisted hydrothermal (MW-HT) synthesis of seeds was performed in two steps as reported by Motuzas et al. [21], using computer controlled Milestone ETHOS 1600 MW oven. The synthesis parameters have been chosen as follows – for the first step T1=80°C, t1=90 min, P1=250W and for the second step T2=160°C, t2=60 min, P2=400W. After synthesis, the suspensions were cooled to 50-60°C and removed from the autoclave. This cooling step occurred by classical convection and lasted typically 30 to 40 min. 55PDF Image | Development of membrane materials for direct methanol fuel cells
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