Chapter II. Aluminum-MOF-air battery (AMA battery)
2.4 Experimental section
Synthesis of Rb-CD-MOF single crystals
In a scintillation vial, 1 mmol γ-Cyclodextrin (1.03g, >98 %, TCI) and 8 mmol Rubidium hydroxide hydrate (0.82 g, 85%, Sigma Aldrich) were dissolved in 20 mL of deionized (DI) water by sonication for 10 minutes. The clear solution was divided evenly into 5 prewashed vials (4 mL per vial). Methanol (ca. 50 mL) was allowed to vapor diffuse into the vials slowly over a period of 4 days. From submillimeter- to millimeter-sized (up to ca. 2*2*1 mm), colorless cubic Rb-CD-MOF single crystals were produced in the vial (Fig. 1c).108109
Preparation of Al anodic electrode
To prepare flat and clean aluminum anode, aluminum surface (99.99%, 0.25 mm thickness, Sigma Aldrich) was grinded with sandpapers which grit size of P1200 and P4000 sequentially, then polished with discs of micro abrasive wetted with diamond suspension (diameter of diamond particles is ca. 3 ~ 9 µm, PRESI) and lubricant (PRESI). The diamond suspension and lubricant stained Al electrode was washed with DI water and acetone. The grinding and polishing process were performed by polishing machine (Mecatech 234, PRESI).
In order to deposit layer of zinc nanoparticles (NPs) embedded polyester (Zn NPs@polyester) as a corrosion inhibitor and separator on the polished Al electrode, following preparation steps were required: 6 wt% mounting wax in 10 mL acetone and zinc nanopowder (20mg, <50nm particle size, ≥99%, Sigma Aldrich) was added in the solution. 2) To disperse the zinc NPs in acetone, the mixed solution was stirred for 24h and then, aggregated particles were filtrated by syringe filter (PTFE, average pore size: 0.45 µm, FluoroporeTM). 3) The polished aluminum foil was put into the solution for 1h and washed by isopropanol and DI water alternately, then dried by blowing nitrogen gas. In this step the Zn NPs@polyester film was deposited on the polished Al. 4) The Zn NPs@polyester coated Al was immersed into 0.1M potassium hydroxide (0.048g, ≥85%, Sigma Aldrich) aqueous solution for 30s. The thickness of Zn NPs@polyester layer on Al is around 10 µm in thickness which was confirmed by a Scanning Electron Microscope (S-4800, Hitach High-Technologies).
Fabrication of Al-MOF-air battery
A single crystal of Rb-CD-MOF was sandwich packed with Zn@polyester coated Al electrode and conductive carbon paste (TED PELLA) (Figure S5). Mostly selected MOF single crystals’
size were ca. 300 µm: 300 µm: 50 µm = width: length: thickness for the Al-MOF-air battery fabrication. For stable positioning of the MOF single crystal on the Al electrode, the MOF crystal was fixed by plastering epoxy (Araldite) only two side walls of the single crystal (Other faces of the cubic single crystal were utilized as channels for water and oxygen adsorption).
Each end of the electrodes (Al and carbon) were connected with copper wire (0.001 in diameter, Alfa Aesar). In order to dry the carbon paste and harden the epoxy, the Al-MOF-air cell was heat at 65℃for 1 hour. Before performing electrochemical measurements, the baked Al-MOF- air cell was filled out vapor from mixed solvent with 70 % methanol and 30 % DI water for an hour with dry air.
Electrochemical measurements
Electrochemical measurements were performed at room temperature using potentiostat (PARSTATMC, Princeton Applied Research) instrument with VersaStudio TM analyst software.
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Performances of Al-MOF air battery were tDested in Schleck flask connected with vaporizing system or vacuum. Fig. S1.
Tafel plots of bare aluminum and Zn NPs@polyester coated aluminum were obtained from Al electrodes as a working electrode, Ag/AgCl as a reference electrode, and platinum wire as a counter electrode. The surfaces were exposed to 0.6 wt% NaCl in aqueous solution (pH 5.6).
Scan rate is 5 mVs-1.110
Figure 2.26 Schematic views and photographs of set up for Al-MOF- air battery. (A and B) For measurement of Al-MOF-air battery perfomance under 4 mTorr vacuum condition and (C and D) under 99% humidified condition with injection of vapor from methanol and water mixture (methanol:water = 70:30).
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