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Anionic Exchange Membrane for Photo-Electrolysis Application

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Anionic Exchange Membrane for Photo-Electrolysis Application polymers Article Anionic Exchange Membrane for Photo-Electrolysis Application Carmelo Lo Vecchio * , Alessandra Carbone * , Stefano Trocino , Irene Gatto , Assunta Patti, Vincenzo Baglio and Antonino Salvatore Aricò Institute for Advanced Energy Technologies “Nicola Giordano”—CNR-ITAE, Via Salita S. Lucia sopra Contesse 5, 98126 Messina, Italy; [email protected] (S.T.); [email protected] (I.G.); [email protected] (A.P.); [email protected] (V.B.); [email protected] (A.S.A.) * Correspondence: [email protected] (C.L.V.); [email protected] (A.C.); Tel.: +39-090-624-288 (C.L.V.); +39-090-624-273 (A.C.) Received: 19 November 2020; Accepted: 12 December 2020; Published: 15 December 2020 Abstract: Tandem photo-electro-chemical cells composed of an assembly of a solid electrolyte membrane and two low-cost photoelectrodes have been developed to generate green solar fuel from water-splitting. In this regard, an anion-exchange polymer–electrolyte membrane, able to separate H2 evolved at the photocathode from O2 at the photoanode, was investigated in terms of ionic conductivity, corrosion mitigation, and light transmission for a tandem photo-electro-chemical configuration. The designed anionic membranes, based on polysulfone polymer, contained positive fixed functionalities on the side chains of the polymeric network, particularly quaternary ammonium species counterbalanced by hydroxide anions. The membrane was first investigated in alkaline solution, KOH or NaOH at different concentrations, to optimize the ion-exchange process. Exchange in 1M KOH solution provided high conversion of the groups, a high ion-exchange capacity (IEC) value of 1.59 meq/g and a hydroxide conductivity of 25 mS/cm at 60 ◦C for anionic membrane. Another important characteristic, verified for hydroxide membrane, was its transparency above 600 nm, thus making it a good candidate for tandem cell applications in which the illuminated photoanode absorbs the highest-energy photons (< 600 nm), and photocathode absorbs the lowest-energy photons. Furthermore, hydrogen crossover tests showed a permeation of H2 through the membrane of less than 0.1%. Finally, low-cost tandem photo-electro-chemical cells, formed by titanium-doped hematite and ionomer at the photoanode and cupric oxide and ionomer at the photocathode, separated by a solid membrane in OH form, were assembled to optimize the influence of ionomer-loading dispersion. Maximum enthalpy (1.7%), throughput (2.9%), and Gibbs energy efficiencies (1.3%) were reached by 2 using n-propanol/ethanol (1:1 wt.) as solvent for ionomer dispersion and with a 25 µL cm− ionomer loading for both the photoanode and the photocathode. Keywords: anion-exchange membrane; ionic conductivity; ionomer; photo-electro-chemical applications; tandem cell 1. Introduction According to the European Strategy Energy Technology (EU SET) plan, by 2050 at least 65% of electric energy should derive from renewable energy sources and, furthermore, CO2 emissions related to the energy production should be reduced by 50%. From this perspective, a drastic reduction in the dependence from fossil fuels could be realized by exploiting all abundant renewable sources that nature reserves: sun [1–3], wind [4,5], water [6,7], and geothermic [8,9]. These technologies have recently experienced large-scale commercialization, and generate electric energy by directly converting the Polymers 2020, 12, 2991; doi:10.3390/polym12122991 www.mdpi.com/journal/polymers Polymers 2020, 12, 2991 2 of 12 energy of renewable sources. However, the main drawbacks are related to their relative intermittence, causing issues in terms of balancing grid processes. Energy produced by the sun in one hour is equal to the amount necessary for the world’s human populationPolymers in2020 one, 12, yearx [10]. Thus, storing energy through the production of solar fuel (hydrogen2 of 12 by water-splitting or hydrocarbons by carbon dioxide reduction) and generating energy from them, Energy produced by the sun in one hour is equal to the amount necessary for the world’s human when it is necessary, has become a “green” challenge [11–14]. population in one year [10]. Thus, storing energy through the production of solar fuel (hydrogen by Photo-electro-chemicalwater-splitting or hydrocarbons (PEC) water-splittingby carbon dioxide (WS) reduction) is a process and generating in which oxygenenergy from and hydrogenthem, evolvewhen at photoanode it is necessary, and has photocathode, become a “green” respectively, challenge [11–14]. using a liquid electrolyte, generally based on concentratedPhoto-electro-chemical hydroxides [15–18 (PEC)]. Effi water-splittingciency and durability (WS) is a toprocess produce in which pure oxygen H2 by photo-electrolysisand hydrogen may beevolve improved at photoanode by employing and photocathode, a solid polymer-electrolyte respectively, using between a liquid electrolyte, the electrodes generally as agas based separator. on This separationconcentrated for hydroxides polymer-electrolyte [15–18]. Efficiency membrane and durability fuel cells (PEMFCs)to produce pure and theirH2 bysubcategories photo-electrolysis [19 –22] has beenmay be known improved for by many employing years a whereas solid polymer-electrolyte the employment between of a the solid-membrane electrodes as a gas electrolyte separator. has beenThis less separation studied forfor polymer-electrolyte PEC applications membrane [23,24]. Itsfuel implementationcells (PEMFCs) and in their a cost-e subcategoriesffective [19– tandem 22] has been known for many years whereas the employment of a solid-membrane electrolyte has PEC architecture, able to capture a significant portion of the solar irradiation, is structured as been less studied for PEC applications [23,24]. Its implementation in a cost-effective tandem PEC photoanode/membrane/photocathode and the working mechanism has been discussed in detail in architecture, able to capture a significant portion of the solar irradiation, is structured as somephotoanode/membrane/photocathode recent work [25,26]. and the working mechanism has been discussed in detail in Assome shown recent in work Figure [25,26].1, photoelectrodes are based on earth-abundant metal oxides such as α-Fe2O3 (hematite)As at shown the photoanode in Figure 1, (PA), photoelectrodes supported are on fluorinebased on tinearth-abundant oxide (FTO) metal substrate oxides and such CuO as α at- the photocathodeFe2O3 (hematite) (PC) deposited at the photoanode on a gas (PA), diffusion supported layer on (GDL) fluorine [27 ].tin The oxide polymer-electrolyte (FTO) substrate and approachCuO requiresat the an ephotocathodeffective interfacial (PC) deposited contact between on a gas polymer-electrolyte diffusion layer (GDL) and [27]. photoelectrodes The polymer-electrolyte able to permit an effiapproachcient ionic requires percolation. an effective interfacial contact between polymer-electrolyte and photoelectrodes able to permit an efficient ionic percolation. FTO/Fe2O3 CuO/GDL membrane 1 M KOH FAA-3 RE WE in H2O ionomer CE SE FAA3-50 1.0 cm 1.0 1.0 cm 1.0 2.2 mm FTO 1 μm CuO 50 μm solid < 1μm Fe O 300 μm GDL 2 3 electrolyte FigureFigure 1. Sketch 1. Sketch of of the the photo-electro-chemical photo-electro-chemical cell cell for for water-splitting. water-splitting. InfiltrationInfiltration of ion of clusters, ion clusters, obtained obtained by dispersing by dispersing the ionomer the ionomer shredded shredded film infilm alcoholic in alcoholic solution, into thesolution, nanostructured into the nanostructured semiconductor’s semiconductor’s layer forms layer an forms extended an extended interface interface with with the metalthe metal oxides. This isoxides. likely facilitatedThis is likely by facilitated the nanocolumnar by the nanocolumnar or nanofibrous or nanofibrous nature of the nature oxide of material,the oxide which material, should allowwhich a more should straightforward allow a more penetration straightforward of the penetrat ion clustersion of the throughout ion clusters the throughout entire thickness the entire of the nanostructuredthickness of electrode. the nanostructured In the sketch, electrode. connections In the sketch, for PEC connections measurements for PEC are measurements represented withare RE represented with RE (reference electrode) and CE (counter electrode) at the photoanode and with WE (reference electrode) and CE (counter electrode) at the photoanode and with WE (working electrode) (working electrode) and SE (sensing electrode) at the photocathode. and SE (sensing electrode) at the photocathode. In summary, the planned research targets for the polymer-electrolyte membrane/ionomer structure are the following: Polymers 2020, 12, 2991 3 of 12 In summary, the planned research targets for the polymer-electrolyte membrane/ionomer structure are the following: Suitable ionic conductivity in the range of 10–50 mS cm 1. • − Low gas crossover. Hydrogen/oxygen permeation smaller than 10 8 mol cm 2 min 1. • − − − High water permeation to allow for proper water management between cathode and anode • according to the main conduction mechanism. Availability of ionomer dispersions to allow for an extension of the ionomer/oxide interface. • Robust mechanical and thermal properties. Capability to sustain high temperatures (up to 85 C). • ◦ Optical transparency in the useful range of wavelengths. • Substantial photo-response of the semiconductor electrodes in contact with the polymer material. • Semiconductor corrosion mitigation properties.
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