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Polymers 2019, 11, 914 7 of 10 change in the slope of the polarization curve is detected, likely due to a difficult water management Polymers 2018, 10, x FOR PEER REVIEW 7 of 10 Paoltymsuercsh201h8i,g1h0, xteFmORpePrEaEtRuRreE.VITEoWbetter elucidate the different contributions to the overall resi7stoifv1it0y, in-operando impedance spectra were recorded while polarizing the cell at 0.6 V. 1,0 200 1,0 200 1.0 1.0 120 120 100 100 0,8 0.8 80 80 60 40 20 0 0. 150 ,8 ,6 ,4 ,2 ,0 N 0 0. 0,6 2 100 0.6 5 100 0 70. 0,4 50 0.4 0 500. 60 40 20 0 0,2 0.2 0 0. 0 0 0 100 200 300 400 M7 500 600 0,0 -2 0 100 200Curren3t0D0ensity4/0m0Acm 500 600 Current Density / mA cm-2 0.0 -2 CurrentD2e00nsity/mAcm300 Current Density / mA cm-2 NM M M2 M5 M 150 0 Figure 5. Fuel cell performances under 31% RH and at T = 80 °C (on the left) or at T= 110 °C (on the Figure 5. Fuel cell performances under 31% RH and at T = 80 ◦C (on the left) or at T= 110 ◦C (on Figure 5. Fuel cell performances under 31% RH and at T = 80 °C (on the left) or at T= 110 °C (on the right). the right). right). Nyquist plots of the iimpedance spectra, recorded during fuel cell operations, are reported in Nyquist plots of the impedance spectra, recorded during fuel cell operations, are reported in Figure6.TThheehihgihghfrefqreuqeunecnyciyntienrtcerpcteopnt othnetrheealraexailsaisxicsonissicdoenrseidaesretdheatsotahlentonta-ellencotnro-edle,cotrhomdeic, Figure 6. The high frequency intercept on the real axis is considered as the total non-electrode, ohmic orehsmisitcanrecseisotfatnhce coefllt,hme ecaenllw, mhieleanthwehliolewthfreqlouwenfcryeqinuteenrcyepitntisermceapint liys mduaeintloytdheuelteoctrhoedel,echtraorgde-, resistance of the cell, meanwhile the low frequency intercept is mainly due to the electrode, charge- cthranrgsfee-rtrraenssisfetarnrceesi[s3ta0n].ce [30]. transfer resistance [30]. 0,2 0,2 0,1 0,1 0,0 0,0 0,0 0,0 0,1 0,1 0,2 0,3 0,4 0,2 0,2 0,1 0,1 0,0 0,0 0,1 0,2 0,3 Z' /Ohm 0,2 real 0,3 Z'real / Ohm 0,4 0,5 0,4 0,5 Z' real φ φ M5 Z'0re,a2l / Ohm 0,3 / Ohm 0,0 0,4 0,0 0,1 N NM2 M2 M7 M5 M7 Figure 6. Impedance spectra recorded at 0.6 V, under 31% RH and at T = 80 ◦C (on the left) or at T= Figu◦ re 6. Impedance spectra recorded at 0.6 V, under 31% RH and at T = 80 °C (on the left) or at T= 110 C (on the right). Frequency range, Φ: 10 KHz–1 Hz. Figure 6. Impedance spectra recorded at 0.6 V, under 31% RH and at T = 80 °C (on the left) or at T= 110 °C (on the right). Frequency range, Ф: 10 KHz - 1Hz. 110 °C (on the right). Frequency range, Ф: 10 KHz - 1Hz. As expected from the fuel cell performances in Figure 5, the composite membranes give rise to lowerAoshemxipcercetseisdtafnrocmes,tchoenffiuremlicnegllapneirmfoprrmovanedcepsrointoFnigcuonredu5,ctihveitcyodmupeotositheemsuepmebraracindeisccgoivmeproisuentdo. As expected from the fuel cell performances in Figure◦ 5, the composite membranes give rise t◦o Alolwsoe,rloowhemr iccharregseistraanncsefse,r croesnifsitramnicnegs aarne oibmseprvoevdedat p80rotCon, ifccoonmdupcatrievdittyo pdluaeintNo atfihoen.suApte1r1a0cidCic, lower ohmic resistances, confirming an improved proton conductivity due to the superacidic tchoemMp2ousanmd.pAlelssoh,olowwsewreclhlacrognetrtorallnesdfecrhraersgiesttarnacnessfearrereosbistearnvced,altlo8w0°inCg,ibfectotmerpcaerlledpetrofoprlmainanNcea.fiOon. compound. Also, lower charge transfer resistances are observed at 80 °C, if compared to plain Nafion. tAhet c1o1n0tr°aCr,y,thuegMe c2hsaargmeptlreansshfoewr rseswisetallnceosn,tmroullcehdlacrhgaerrgtehatrnanNsaffieronreistsisetlaf,nacree, aslslowciaintegdbtoetthere Mce5ll At 110 °C, the M2 sample shows well controlled charge transfer resistance, allowing better cell spaemrfpolremaatnhcieg.hOtenmthpercaotnutrrea,reyv,ehnutgheouchgahrgoeotdrapnrsofetornrecsoinstdauncteisv,itmyuischprleasregrevretdh,ans Nevaifdieontiftrsoemlf, tahre performance. On the contrary, huge charge transfer resistances, much larger than Nafion itself, are ianstseorcieaptetdatohtighhe Mfre5qsuaemnpclye. aTthiisgehxtpelmaipnetrhaetupreo,oervbeenhtahvoiuogrhogf othoedMpr5otsoanmcpolnediuncthiveitfyueisl pcerellsteersvteadt, assoc◦iatedtotheM5sampleathightemperature,eventhoughgoodprotonconductivityispreserved, 1a1s0evCid,ewnhtefreomstrtohnegineltecrtcreopdteaptohliagrhizfarteiqounesnwcyer.eTahlirseaedxpyloaibnsethrveepdo.orbehavioroftheM5samplein as evident from the intercept at high frequency. This explain the poor behavior of the M5 sample in the fuOevlecrealllt,etshteaitn1o1r0ga°Cni,cwahdedrietisvteroinsgfoeulencdtrtoodaeffpeocltadriizffaetrioenst iwmepreoratlarneatdfeyaotubrsesrvoefdt.he composite the fuel cell test at 110 °C, where strong electrode polarizations were already observed. membOrvaenrea,ltl,htahtearineo(ir)gtahneicpraodtdointicvoenidsufoctuivnidtyt,o(iai)fftehcethdyifdfrearteinotnidmepgorerteaanntdfe(aiitiu)rtehseorfesthisetivcoitmy patosthite Overall, the inorganic additive is found to affect different important features of the composite membrane/,etlheactraordeei)inthterfparcoet.onWciothndreuscptievcittyto,itih)itshelahttyedrrpaotiionnt,daebgerenefiancidaliieiff)ethcetorefstihsetivinitoyrgatanthice membrane, that are i) the proton conductivity, ii) the hydration degree and iii) the resistivity at the amdedmitibvreanone/tehlecrteroladxeatinotnerpfraoccee.sWsoitfhNraefisopnecwtittohthemisplaetrtaetrurpeo,ianvto,iadibnegnoefricaitalleaesfftercetdoufcitnhgesihnroirngkangiec membrane/electrode interface. With respect to this latter point, a beneficial effect of the inorganic oafdtdhietimveemonbrathne,sreolaenxasutiroingparobceettsesrionfteNrfafcieonconwtiatchtwteimthptehreaetulercet,roadveosi,dwinagsaolreadtyleoabssterveedduc[3in1g]. additive on the relaxation process of Nafion with temperature, avoiding or at least reducing Isnhtrhiniskwagoerko,fththeecomnetmriburatinoen, osfoseunlfsauteridntgitanbiaetitnerteirnmtesrfoafcceelclocnhtarcgtewtriathnstfheer perleocpterortdies,anwdaselaeclrteroadey shrinkage of the membrane, so ensuring a better interface contact with the electrodes, was already pooblsaerivzeadtio[n3s1]i.s Ifnoutnhdis two oprlka,y tahecrucocniatlrirbouletioant hoifghsutlefmatpederatittuarneianind itsersmtrsonogflycedllepcehnadrgeenttroanstfheer observed [31]. In this work, the contribution of sulfated titania in terms of cell charge transfer fiplrloerpecortniecsenatnradtieolne.ctrode polarizations is found to play a crucial role at high temperature and is properties and electrode polarizations is found to play a crucial role at high temperature and is strongly dependent on the filler concentration. strongly dependent on the filler concentration. 4. Conclusions 4. Conclusions The properties of composite Nafion membranes with a sulfated titania additive were The properties of composite Nafion membranes with a sulfated titania additive were investigated. A new template-driven synthesis was developed to obtain highly acidic inorganic investigated. A new template-driven synthesis was developed to obtain highly acidic inorganic 8 6 4 2 0 N 0 100 400 0 100 M5 200 300 NM2 M5 M2 φ φ M5 M2 N NM2 M5 400 Power Density / mW cm-2 Power Density / mW cm-2 Power Density / mW cm-2 Power Density / mW cm-2 -Z'' / Ohm Cell Voltage / V imm / Ohm -Z'' imm -Z'' / Ohm imm -Z'' / Ohm imm Cell Voltage / V Cell Voltage / V Cell Voltage / VPDF Image | Polymer Electrolyte Membranes Based on Nafion Fuel Cell
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