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Izindleko eziphakeme kakhulu zawo wonke amabhethri e-vanadium flow-through redox (VRFBs) zikhawulela ukusetshenziswa kwawo okusabalele.Ukuthuthukisa i-kinetics of electrochemical reactions kuyadingeka ukuze kwandiswe amandla athile kanye nokusebenza kahle kwamandla kwe-VRFB, ngaleyo ndlela kwehliswe izindleko ze-kWh ze-VRFB.Kulo msebenzi, i-hydrothermally synthesized hydrated tungsten oxide (HWO) nanoparticles, i-C76 ne-C76/HWO, yafakwa kuma-electrode endwangu ye-carbon futhi yahlolwa njengama-electrocatalysts ku-VO2+/VO2+ redox reaction.I-Field emission scanning electron microscopy (FESEM), i-energy dispersive X-ray spectroscopy (EDX), i-high-resolution transmission electron microscopy (HR-TEM), i-X-ray diffraction (XRD), i-X-ray photoelectron spectroscopy (XPS), i-infrared i-Fourier transform Spectroscopy (FTIR) nezilinganiso ze-engeli yokuxhumana.Kutholwe ukuthi ukungezwa kwe-C76 fullerenes ku-HWO kungathuthukisa i-electrode kinetics ngokwandisa ukuhanjiswa kukagesi nokuhlinzeka ngamaqembu asebenza nge-oxidized endaweni yayo, ngaleyo ndlela kukhuthaze ukusabela kwe-VO2+/VO2+ redox.Inhlanganisela ye-HWO/C76 (50 wt% C76) ibonakale iyisinqumo esingcono kakhulu sokusabela kwe-VO2+/VO2+ nge-ΔEp ye-176 mV, kuyilapho indwangu yekhabhoni engelashiwe (UCC) ibingu-365 mV.Ukwengeza, inhlanganisela ye-HWO/C76 ibonise umphumela obalulekile wokuvimbela ekuphenduleni kwe-chlorine ye-parasitic ngenxa yeqembu elisebenzayo le-W-OH.
Imisebenzi yabantu eshubile kanye nenguquko esheshayo yezimboni kuholele esidingweni esikhulu ngokungenakuvinjelwa sikagesi, esikhula cishe ngama-3% ngonyaka1.Emashumini eminyaka, ukusetshenziswa kabanzi kwezibaso ezimbiwa phansi njengomthombo wamandla kuye kwaholela ekukhishweni kwesisi esibamba ukushisa okubangela ukufudumala kwembulunga yonke, ukungcoliswa kwamanzi nomoya, okusongela yonke imvelo.Ngenxa yalokho, ukungena komoya ohlanzekile novuselelekayo kanye namandla elanga kulindeleke ukuthi kufinyelele ku-75% wawo wonke ugesi ngo-20501. Kodwa-ke, lapho isabelo sikagesi esivela emithonjeni evuselelekayo sidlula ama-20% engqikithi yokuphehlwa kukagesi, igridi iba nokungazinzi.
Phakathi kwazo zonke izinhlelo zokugcina amandla njenge-hybrid vanadium redox flow battery2, ibhethri ye-vanadium redox flow battery (VRFB) ithuthuke ngokushesha kakhulu ngenxa yezinzuzo zayo eziningi futhi ibhekwa njengesixazululo esingcono kakhulu sokugcina amandla isikhathi eside (cishe iminyaka engu-30).) Izinketho ezihlanganiswe namandla avuselelekayo4.Lokhu kungenxa yokuhlukaniswa kwamandla namandla, impendulo esheshayo, impilo ende yesevisi, kanye nezindleko eziphansi zonyaka ezilinganiselwa ku-$65/kWh uma kuqhathaniswa no-$93-140/kWh wamabhethri e-Li-ion nawe-lead-acid kanye nama-dollar angu-279-420 ase-US kWh ngayinye.ibhethri ngokulandelana 4.
Kodwa-ke, ukuthengisa kwabo ngezinga elikhulu kusavinjelwa izindleko zabo ezinkulu zesistimu, ikakhulukazi ngenxa yezitaki zamaseli4,5.Ngakho-ke, ukuthuthukisa ukusebenza kwesitaki ngokwandisa i-kinetics yokusabela kwengxenye yengxenye emibili kunganciphisa usayizi wesitaki futhi ngaleyo ndlela kunciphise izindleko.Ngakho-ke, ukudluliswa kwe-electron okusheshayo endaweni ye-electrode kuyadingeka, okuncike ekuklanyeni, ukwakheka kanye nesakhiwo se-electrode futhi kudinga ukulungiselelwa ngokucophelela6.Naphezu kokuzinza okuhle kwamakhemikhali kanye ne-electrochemical kanye ne-conductivity kagesi enhle ye-carbon electrode, i-kinetics yabo engaphenduliwe ivilapha ngenxa yokungabikho kwamaqembu okusebenza kwe-oksijeni kanye ne-hydrophilicity7,8.Ngakho-ke, ama-electrocatalyst ahlukahlukene ahlanganiswa nama-electrode asekelwe ku-carbon, ikakhulukazi ama-carbon nanostructures nama-oxide ensimbi, ukuze kuthuthukiswe i-kinetics yawo womabili ama-electrode, ngaleyo ndlela kwandiswe i-kinetics ye-electrode ye-VRFB.
Ngaphezu komsebenzi wethu wangaphambilini ku-C76, siqale sabika umsebenzi omuhle kakhulu we-electrocatalytic wale fullerene ye-VO2+/VO2+, ukudluliswa kwenkokhiso, uma kuqhathaniswa nendwangu yekhabhoni ephethwe ukushisa nengaphathwanga.Ukumelana kwehle ngo-99.5% no-97%.Ukusebenza kwe-catalytic yezinto zekhabhoni zokusabela kwe-VO2+/VO2+ uma kuqhathaniswa ne-C76 kuboniswa kuThebula S1.Ngakolunye uhlangothi, ama-oxide amaningi ensimbi afana ne-CeO225, ZrO226, MoO327, NiO28, SnO229, Cr2O330 kanye ne-WO331, 32, 33, 34, 35, 36, 37 asetshenzisiwe ngenxa yokukhula kwawo okumanzi kanye nokusebenza komoyampilo omningi., 38. iqembu.Umsebenzi we-catalytic walawa ma-oxide ensimbi ekuphenduleni kwe-VO2+/VO2+ uvezwa kuThebula S2.I-WO3 isetshenziswe enanini elibalulekile lemisebenzi ngenxa yezindleko zayo eziphansi, ukuzinza okuphezulu kwemithombo ye-acidic, kanye nomsebenzi ophezulu we-catalytic31,32,33,34,35,36,37,38.Nokho, ukuthuthukiswa kwe-cathodic kinetics ngenxa ye-WO3 akubalulekile.Ukuze uthuthukise ukuqhutshwa kwe-WO3, umphumela wokusebenzisa i-tungsten oxide encishisiwe (W18O49) emsebenzini we-cathodic uhlolwe38.I-Hydrated tungsten oxide (HWO) ayikaze ihlolwe ezinhlelweni ze-VRFB, nakuba ibonisa umsebenzi owengeziwe ezinhlelweni ze-supercapacitor ngenxa yokusabalalisa kwe-cation okusheshayo uma kuqhathaniswa ne-anhydrous WOx39,40.Ibhethri lesizukulwane sesithathu le-vanadium redox eligeleza lisebenzisa i-electrolyte ye-asidi exubile eyakhiwe i-HCl ne-H2SO4 ukuze kuthuthukiswe ukusebenza kwebhethri futhi kuthuthukiswe ukunyibilika nokuzinza kwama-ion e-vanadium ku-electrolyte.Kodwa-ke, i-parasitic chlorine evolution reaction isibe enye yezinto ezimbi zesizukulwane sesithathu, ngakho ukucinga izindlela zokuvimbela ukusabela kokuhlolwa kwe-chlorine sekugxilwe kumaqembu amaningana ocwaningo.
Lapha, ukuhlolwa kokusabela kwe-VO2+/VO2+ kwenziwa kuzinhlanganisela ze-HWO/C76 ezifakwe kuma-electrode endwangu ye-carbon ukuze kutholwe ibhalansi phakathi kokuhamba kukagesi kwezinhlanganisela kanye ne-redox kinetics yendawo ye-electrode kuyilapho kucindezela ukuvela kwe-parasitic chlorine.impendulo (CER).Ama-nanoparticles e-tungsten oxide (HWO) afakwe emanzini ahlanganiswa ngendlela elula ye-hydrothermal.Izivivinyo zenziwe nge-electrolyte ye-asidi exubile (H2SO4/HCl) ukuze kulingise isizukulwane sesithathu i-VRFB (G3) ukuze kube nokusebenziseka kanye nokuphenya umthelela we-HWO ekuphenduleni kwe-parasitic chlorine evolution.
I-Vanadium(IV) sulfate hydrate (VOSO4, 99.9%, Alfa-Aeser), sulfuric acid (H2SO4), hydrochloric acid (HCl), dimethylformamide (DMF, Sigma-Aldrich), polyvinylidene fluoride (PVDF, Sigma)-Aldrich), i-sodium Tungstenphild-Aldrich, i-sodium Tungstenphild-Aldrich, i-sodium Tungstenphild, i-Sigstenphild 4, i-Sigstenphild 4, i-Sigma-Aldrich Indwangu ELAT (Fuel Cell Store) isetshenziswe kulolu cwaningo.
I-tungsten oxide (HWO) ene-Hydrated yalungiselelwa ukusabela kwe-hydrothermal 43 lapho u-2 g kasawoti we-Na2WO4 wancibilika ku-12 ml we-H2O ukuze kunikezwe isixazululo esingenambala, bese kwengezwa u-12 ml we-2 M HCl ngokudonsela phansi ukuze unikeze ukumiswa okuphuzi okuphaphathekile.I-slurry yafakwa ku-autoclave yensimbi engenasici e-Teflon futhi yagcinwa kuhhavini ku-180 ° C. amahora angu-3 ukusabela kwe-hydrothermal.Okusele kuqoqwe ngokuhlunga, kugezwe izikhathi ezi-3 nge-ethanol namanzi, yomiswa kuhhavini ku-70 ° C amahora angu-3, ​​bese i-triturated ukunikeza i-HWO powder eluhlaza okwesibhakabhaka.
Ama-electrode endwangu yekhabhoni etholiwe (engaphathwanga) asetshenziswe njengoba enjalo noma aphathwe ukushisa esithandweni somlilo esingu-450°C emoyeni ngezinga lokushisa elingu-15 ºC/min amahora angu-10 ukuze kutholwe ama-CC alashiwe (TCC).njengoba kuchazwe esihlokweni esandulele24.I-UCC ne-TCC zasikwa zaba ama-electrode acishe abe ngu-1.5 cm ububanzi no-7 cm ubude.Ukumiswa kwe-C76, HWO, HWO-10% C76, HWO-30% C76 kanye ne-HWO-50% C76 kwalungiselelwa ngokwengeza u-20 mg .% (~2.22 mg) we-PVDF binder ku-~1 ml DMF futhi sonicated ihora elingu-1 ukuze kuthuthukiswe ukufana.I-2 mg yezinhlanganisela ze-C76, i-HWO ne-HWO-C76 isetshenziswe ngokulandelana endaweni ye-electrode esebenzayo ye-UCC ecishe ibe ngu-1.5 cm2.Wonke ama-catalyst alayishwa kuma-electrode e-UCC futhi i-TCC yasetshenziselwa izinjongo zokuqhathanisa kuphela, njengoba umsebenzi wethu wangaphambilini wabonisa ukuthi ukwelapha ukushisa kwakungadingeki24.Ukulungiswa kombono kwafinyelelwa ngokuxubha u-100 µl wokumiswa (umthwalo ongu-2 mg) ukuze kube nomphumela olinganayo.Khona-ke wonke ama-electrode omiswa kuhhavini ku-60 ° C. ubusuku bonke.Ama-electrode akalwa phambili nangemuva ukuze kuqinisekiswe ukulayishwa kwesitoko okunembile.Ukuze ube nendawo ethile yejometri (~ 1.5 cm2) futhi uvimbele ukuphakama kwe-vanadium electrolyte ku-electrode ngenxa yomphumela we-capillary, ungqimba omncane weparafini wasetshenziswa phezu kwezinto ezisebenzayo.
I-Field emission scanning electron microscopy (FESEM, Zeiss SEM Ultra 60, 5 kV) yasetshenziswa ukubuka i-HWO surface morphology.I-spectrometer ye-X-ray ehlakaza amandla efakwe i-Feii8SEM (EDX, Zeiss Inc.) yasetshenziswa ukwenza imephu izici ze-HWO-50%C76 kuma-electrode e-UCC.Isibonakhulu se-electron edlulisa ukulungiswa okuphezulu (HR-TEM, JOEL JEM-2100) esebenza ngamandla kagesi asheshayo angama-200 kV yasetshenziselwa ukwenza isithombe sezinhlayiya ze-HWO ezinokucaca okuphezulu namaringi e-diffraction.Isofthiwe ye-Crystallography Toolbox (CrysTBox) isebenzisa umsebenzi we-ringGUI ukuze ihlaziye iphethini yokuhlukanisa indandatho ye-HWO futhi iqhathanise imiphumela nephethini ye-XRD.Isakhiwo ne-graphitization ye-UCC ne-TCC kwahlaziywa nge-X-ray diffraction (XRD) ngesilinganiso sokuskena esingu-2.4°/min kusuka ku-5° kuya ku-70° nge-Cu Kα (λ = 1.54060 Å) kusetshenziswa i-Panalytical X-ray diffractometer (Model 3600).I-XRD ibonise ukwakheka kwekristalu nesigaba se-HWO.Isofthiwe ye-PANalytical X'Pert HighScore isetshenziselwe ukufanisa iziqongo ze-HWO namamephu we-tungsten oxide atholakala kusizindalwazi45.Imiphumela ye-HWO iqhathaniswe nemiphumela ye-TEM.Ukwakheka kwamakhemikhali nesimo samasampuli e-HWO kunqunywe i-X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi, ThermoScientific).Isofthiwe ye-CASA-XPS (v 2.3.15) isetshenziselwe ukukhishwa kwe-deconvolution nokuhlaziya idatha.Ukuze kutholwe amaqembu asebenza phezulu e-HWO ne-HWO-50% C76, izilinganiso zenziwe kusetshenziswa i-Fourier transform infrared spectroscopy (FTIR, Perkin Elmer spectrometer, kusetshenziswa i-KBr FTIR).Imiphumela yaqhathaniswa nemiphumela ye-XPS.Izilinganiso zama-engeli othintana naye (KRUSS DSA25) nazo zasetshenziswa ukukhombisa ukumanzisa kwama-electrode.
Kuzo zonke izilinganiso ze-electrochemical, indawo yokusebenza ye-Biologic SP 300 yasetshenziswa.I-Cyclic voltammetry (CV) kanye ne-electrochemical impedance spectroscopy (EIS) zisetshenziswe ukutadisha i-electrode kinetics ye-VO2+/VO2+ redox reaction kanye nomthelela we-reagent diffusion (VOSO4(VO2+)) kwizinga lokusabela.Zombili izindlela zisebenzisa iseli le-electrode emithathu elinengxube ye-electrolyte engu-0.1 M VOSO4 (V4+) ku-1 M H2SO4 + 1 M HCl (ingxube yama-asidi).Yonke idatha ye-electrochemical eyethulwa i-IR ilungisiwe.Ikhoyili ye-calomel egcwele (SCE) kanye nekhoyili yeplatinamu (Pt) kwasetshenziswa njengereferensi ne-counter electrode, ngokulandelana.Ku-CV, izilinganiso zokuskena (ν) zokungu-5, 20, kanye no-50 mV/s zisetshenziswe efasiteleni elinamandla le-VO2+/VO2+ le-(0–1) V vs. SCE, bese lilungiswa ukuze i-SHE ihlele (VSCE = 0.242 V vs. HSE) .Ukutadisha ukugcinwa komsebenzi we-electrode, ama-CV angama-cyclic aphindaphindiwe enziwa ngo-ν 5 mV/s we-UCC, TCC, UCC-C76, UCC-HWO, kanye ne-UCC-HWO-50% C76.Ezilinganisweni ze-EIS, ububanzi befrikhwensi ye-VO2+/VO2+ redox reaction kwaba ngu-0.01-105 Hz, futhi ukuphazamiseka kwamandla kagesi ku-open-circuit voltage (OCV) kwaba ngu-10 mV.Ukuhlolwa ngakunye kwaphindwa izikhathi ezingu-2-3 ukuze kuqinisekiswe ukuhambisana kwemiphumela.Izilinganiso zesilinganiso ezingafani (k0) zitholwe ngendlela ye-Nicholson46,47.
I-tungsten oxide enamanzi (HVO) yenziwe ngempumelelo ngendlela ye-hydrothermal.Isithombe se-SEMI-1a ibonisa ukuthi i-HWO efakiwe iqukethe amaqoqo ama-nanoparticles anosayizi kububanzi obungu-25-50 nm.
Iphethini ye-X-ray diffraction ye-HWO ibonisa iziqongo (001) kanye (002) ku-~23.5° kanye no-~47.5°, ngokulandelana, okuyisici se-nonstoichiometric WO2.63 (W32O84) (PDF 077–0810, a = 21.4 Å Å3 = Å γ = 1, b Å 8 = , b Å 8 = , b Å 8 = , b Å 8 = , b = 1 = 1 = 1 = 1. 90 °), ohambelana nombala wabo oluhlaza okwesibhakabhaka ocacile (Fig. 1b) 48.49.Ezinye iziqongo ezicishe zibe ngu-20.5°, 27.1°, 28.1°, 30.8°, 35.7°, 36.7° kanye no-52.7° zabelwe (140), (620), (350), (720), (740), (560°).) ) kanye (970) nezindiza ze-diffraction ze-orthogonal ukuya ku-WO2.63, ngokulandelanayo.Indlela efanayo yokwenziwa yasetshenziswa nguSongara et al.43 ukuze bathole umkhiqizo omhlophe, obalulwe ukuba khona kwe-WO3(H2O)0.333.Kodwa-ke, kulo msebenzi, ngenxa yezimo ezihlukene, kutholwe umkhiqizo ompunga oluhlaza okwesibhakabhaka, obonisa ukuthi i-WO3 (H2O) 0.333 (PDF 087-1203, a = 7.3 Å, b = 12.5 Å, c = 7 .7 Å, α = β = γ = 90 °) nefomu elincishisiwe le-oxide.Ukuhlaziywa kwe-semiquantitative kusetshenziswa isofthiwe ye-X'Pert HighScore kubonise u-26% WO3(H2O)0.333:74% W32O84.Njengoba i-W32O84 iqukethe i-W6+ ne-W4+ (1.67:1 W6+:W4+), okuqukethwe okulinganiselwe kwe-W6+ ne-W4+ cishe ku-72% W6+ no-28% W4+, ngokulandelanayo.Izithombe ze-SEM, i-1-second XPS spectra ezingeni le-nucleus, izithombe ze-TEM, i-FTIR spectra, kanye ne-Raman spectra yezinhlayiya ze-C76 zethulwe esihlokweni sethu sangaphambilini.Ngokusho kukaKawada et al.,50,51 X-ray diffraction ye-C76 ngemva kokususwa kwe-toluene kubonise isakhiwo se-monoclinic se-FCC.
Izithombe ze-SEM ku-fig.I-2a kanye ne-b ibonisa ukuthi i-HWO ne-HWO-50% C76 zifakwe ngempumelelo phakathi naphakathi kwama-carbon fibers we-electrode ye-UCC.Amamephu wesici se-EDX we-tungsten, ikhabhoni, nomoya-mpilo ku-SEM izithombe kufig.2c ikhonjisiwe ku fig.I-2d-f ebonisa ukuthi i-tungsten nekhabhoni kuxutshwe ngokulinganayo (ibonisa ukusatshalaliswa okufanayo) phezu kwayo yonke indawo ye-electrode futhi nenhlanganisela ayifakwanga ngokufanayo ngenxa yemvelo yendlela yokubeka.
Izithombe ze-SEM zezinhlayiya ezifakiwe ze-HWO (a) nezinhlayiyana ze-HWO-C76 (b).Imephu ye-EDX ku-HWO-C76 elayishwe ku-UCC isebenzisa indawo esesithombeni (c) ibonisa ukusatshalaliswa kwe-tungsten (d), ikhabhoni (e), nomoya-mpilo (f) kusampula.
I-HR-TEM isetshenziselwe ukuthwebula isithombe sokukhulisa okuphezulu nolwazi lwecrystallographic (Umfanekiso 3).I-HWO ikhombisa i-nanocube morphology njengoba kukhonjisiwe ku-Fig. 3a futhi ngokucacile ku-Fig. 3b.Ngokukhulisa i-nanocube ye-diffraction yezindawo ezikhethiwe, umuntu angabona ngeso lengqondo isakhiwo se-grating nezindiza ze-diffraction ezanelisa umthetho we-Bragg, njengoba kuboniswe ku-Fig. 3c, okuqinisekisa ubucwebe bezinto.Esihlokweni esikuFig. 3c sikhombisa ibanga d 3.3 Å elihambisana nezindiza ze-diffraction (022) kanye (620) ezitholakala kuzigaba ze-WO3(H2O)0.333 kanye ne-W32O84, ngokulandelana kwazo43,44,49.Lokhu kuhambisana nokuhlaziywa kwe-XRD okuchazwe ngenhla (I-Fig. 1b) njengoba ibanga lendiza egayiwe elibonwayo d (I-Fig. 3c) lihambisana nenani eliphakeme kakhulu le-XRD kusampula ye-HWO.Izindandatho zesampula nazo zikhonjiswe emkhiwaneni.3d, lapho indandatho ngayinye ihambisana nendiza ehlukile.Izindiza ze-WO3(H2O) 0.333 kanye ne-W32O84 zinemibala emhlophe neluhlaza okwesibhakabhaka, ngokulandelana, futhi iziqongo zazo ezihambisanayo ze-XRD nazo ziboniswa ku-Fig. 1b.Iringi yokuqala ekhonjiswe kumdwebo wendandatho ihambisana nenani eliphakeme lokuqala elimakiwe kwiphethini ye-x-ray yendiza yokuhluka (022) noma (620).Kusukela ku-(022) kuya ku-(402) amasongo, amanani we-d-spacing angu-3.30, 3.17, 2.38, 1.93, kanye no-1.69 Å, ngokuhambisana namanani e-XRD angu-3.30, 3.17, 2, 45, 1.93.kanye no-1.66 Å, okulingana no-44, 45, ngokulandelana.
(a) Isithombe se-HR-TEM se-HWO, (b) sibonisa isithombe esinwetshiwe.Izithombe zezindiza ezisanhlamvu ziboniswa ku-(c), inset (c) sibonisa isithombe esikhulisiwe sezindiza kanye ne-pitch d engu-0.33 nm ehambisana nezindiza (002) kanye (620).(d) Iphethini yeringi ye-HWO ebonisa izindiza ezihlotshaniswa ne-WO3(H2O)0.333 (emhlophe) ne-W32O84 (eluhlaza okwesibhakabhaka).
Ukuhlaziywa kwe-XPS kwenziwa ukuze kunqunywe ikhemistri engaphezulu nesimo se-oxidation se-tungsten (Izibalo S1 no-4).Ububanzi obubanzi bokuskena be-XPS be-HWO ehlanganisiwe buboniswa kuMfanekiso S1, okubonisa ukuba khona kwe-tungsten.I-spectra ye-XPS yokuskena encane yezinga eliyinhloko le-W 4f ne-O 1s iboniswa ku-Fig.4a kanye b, ngokulandelana.I-spectrum ye-W 4f ihlukana ibe ama-spin-orbit double ahambisana namandla abophayo wesimo se-W se-oxidation.kanye no-W 4f7/2 kokuthi 36.6 kanye no-34.9 eV kuyisici sesimo se-W4+ esingu-40, ngokulandelanayo.)0.333.Idatha efakiwe ibonisa ukuthi amaphesenti e-athomu e-W6+ ne-W4+ angu-85% no-15%, ngokulandelana, aseduze namanani alinganiselwe kusukela kudatha ye-XRD kucatshangelwa umehluko phakathi kwalezi zindlela ezimbili.Zombili izindlela zinikeza ulwazi lobuningi ngokunemba okuphansi, ikakhulukazi i-XRD.Futhi, lezi zindlela ezimbili zihlaziya izingxenye ezihlukene zezinto ezibonakalayo ngoba i-XRD iyindlela yobuningi kuyilapho i-XPS iyindlela engaphezulu esondela kuma-nanometer ambalwa kuphela.I-spectrum ye-O 1s ihlukaniswe yaba iziqongo ezimbili ku-533 (22.2%) kanye ne-530.4 eV (77.8%).Eyokuqala ihambisana ne-OH, kanti eyesibili ihambisana ne-oxygen bond ku-lattice ku-WO.Ukuba khona kwamaqembu e-OH asebenzayo kuhambisana nezakhiwo ze-hydration ze-HWO.
Ukuhlaziywa kwe-FTIR kuphinde kwenziwa kulawa masampuli amabili ukuhlola ukuba khona kwamaqembu asebenzayo kanye nokuxhumanisa ama-molecule amanzi esakhiweni se-HWO esinamanzi.Imiphumela ibonisa ukuthi isampula ye-HWO-50% C76 kanye nemiphumela ye-FT-IR HWO ibonakala ifana ngenxa yokuba khona kwe-HWO, kodwa ukushuba kweziqongo kuyahluka ngenxa yenani elihlukile lesampula elisetshenziswa ekulungiseleleni ukuhlaziywa (Fig. 5a).) I-HWO-50% C76 ibonisa ukuthi zonke iziqongo, ngaphandle kwesiqongo se-tungsten oxide, zihlobene ne-fulerene 24. Okuningiliziwe ku-fig.I-5a ibonisa ukuthi womabili amasampula abonisa ibhendi ebanzi eqinile kakhulu ku-~710/cm okubalulwe ama-oscillations anwebekayo e-OWO esakhiweni se-lattice se-HWO, nehlombe eliqinile kokuthi ~840/cm okubalulwe ku-WO.Ngokudlidliza okunwebekayo, ibhande elicijile elicishe libe ngu-1610/cm libangelwa ukudlidliza okugobayo kwe-OH, kuyilapho ibhendi yokumunca ebanzi ecishe ibe ngu-3400/cm ibangelwa ukudlidliza kwe-OH kumaqembu e-hydroxyl43.Le miphumela ihambisana ne-XPS spectra kumaFig.4b, lapho amaqembu asebenzayo e-WO anganikeza amasayithi asebenzayo wokusabela kwe-VO2+/VO2+.
Ukuhlaziywa kwe-FTIR kwe-HWO ne-HWO-50% C76 (a), kubonise amaqembu asebenzayo kanye nezilinganiso ze-engeli yokuxhumana (b, c).
Iqembu le-OH lingakwazi futhi ukugqugquzela ukusabela kwe-VO2+/VO2+, kuyilapho likhulisa i-hydrophilicity ye-electrode, ngaleyo ndlela likhuthaze izinga lokusatshalaliswa nokudluliswa kwama-electron.Njengoba kukhonjisiwe, isampula ye-HWO-50% C76 ibonisa ukuphakama okwengeziwe kwe-C76.Iziqongo kokuthi ~2905, 2375, 1705, 1607, and 1445 cm3 zingabelwa ukudlidliza okunwebekayo okungu-CH, O=C=O, C=O, C=C, kanye ne-CO, ngokulandelana.Kuyaziwa ukuthi amaqembu asebenza komoyampilo C=O kanye ne-CO angasebenza njengezikhungo ezisebenzayo zokusabela kwe-redox ye-vanadium.Ukuze kuhlolwe futhi kuqhathaniswe ukumanzisa kwama-electrode amabili, izilinganiso ze-engeli yokuxhumana zithathwe njengoba kuboniswe ku-Fig. 5b, c.I-electrode ye-HWO yamunca ngokushesha amaconsi amanzi, okubonisa ukuthi i-superhydrophilicity ngenxa yamaqembu asebenzayo we-OH atholakalayo.I-HWO-50% C76 i-hydrophobic kakhulu, ine-engeli yokuxhumana cishe engu-135° ngemva kwemizuzwana engu-10.Kodwa-ke, ezilinganisweni ze-electrochemical, i-electrode ye-HWO-50% C76 ibe manzi ngokuphelele ngaphansi komzuzu.Izilinganiso zokumanzisa ziyahambisana nemiphumela ye-XPS ne-FTIR, okubonisa ukuthi amaqembu e-OH engeziwe endaweni ye-HWO ayenza ibe ne-hydrophilic kakhulu.
Ukusabela kwe-VO2+/VO2+ kwe-HWO kanye ne-HWO-C76 nanocomposites kwahlolwa futhi kwakulindeleke ukuthi i-HWO izocindezela ukuvela kwe-chlorine ekuphenduleni kwe-VO2+/VO2+ ku-asidi exubile, futhi i-C76 izophinde iqhubekisele phambili ukusabela okufunayo kwe-VO2+/VO2+ redox.%, 30%, kanye no-50% C76 ekumisweni kwe-HWO futhi i-CCC ifakwe kuma-electrode anokulayisha okuphelele okungaba ngu-2 mg/cm2.
Njengoba kuboniswe emkhiwaneni.6, i-kinetics yokusabela kwe-VO2+/VO2+ endaweni ye-electrode yahlolwa yi-CV ku-electrolyte ene-asidi exubile.Ama-currents aboniswa njenge-I/Ipa ukuze kuqhathaniswe kalula i-ΔEp ne-Ipa/Ipc kuma-catalyst ahlukene ngqo kugrafu.Idatha yendawo yamanje ikhonjisiwe kuMfanekiso 2S.Emkhiwaneni.Umfanekiso 6a ubonisa ukuthi i-HWO inyusa kancane izinga lokudlulisa i-electron ye-VO2+/VO2+ redox yokusabela endaweni ye-electrode futhi icindezela ukusabela kwe-parasitic chlorine evolution.Kodwa-ke, i-C76 inyusa kakhulu izinga lokudlulisa ama-electron futhi igqugquzela ukusabela kokuvela kwe-chlorine.Ngakho-ke, inhlanganisela eyenziwe kahle ye-HWO ne-C76 kulindeleke ukuthi ibe nomsebenzi ongcono kakhulu kanye nekhono elikhulu kakhulu lokuvimbela ukusabela kokuvela kwe-chlorine.Kutholakale ukuthi ngemva kokwandisa okuqukethwe kwe-C76, umsebenzi we-electrochemical we-electrode uthuthukisiwe, njengoba kuboniswa ukwehla kwe-ΔEp kanye nokwanda kwesilinganiso se-Ipa / Ipc (Ithebula S3).Lokhu kuphinde kwaqinisekiswa amanani e-RCT akhishwe esakhiweni se-Nyquist ku-Fig. 6d (Ithebula S3), atholwe ehla ngokuqukethwe okwandayo kwe-C76.Le miphumela ibuye ihambisane nocwaningo luka-Li, lapho ukungezwa kwekhabhoni ye-mesoporous ku-WO3 e-mesoporous kubonise izindlela ezithuthukisiwe zokudlulisa ukushaja ku-VO2+/VO2+35.Lokhu kubonisa ukuthi ukusabela okuqondile kungase kuncike kakhulu ku-electrode conductivity (C=C bond) 18, 24, 35, 36, 37. Lokhu kungase futhi kube ngenxa yoshintsho lwejometri yokuxhumanisa phakathi kwe-[VO(H2O)5]2+ kanye ne- [VO2(H2O)4]+, i-C76 inciphisa ukusabela kwe-tishu overvoltage.Nokho, lokhu kungase kungenzeki ngama-electrode e-HWO.
(a) Ukuziphatha kwe-cyclic voltammetric (ν = 5 mV/s) yokusabela kwe-VO2+/VO2+ ye-UCC nenhlanganisela ye-HWO-C76 enezilinganiso ezihlukile ze-HWO:C76 ku-0.1 M VOSO4/1 M H2SO4 + 1 M HCl electrolyte.(b) I-Randles-Sevchik kanye (c) nendlela ye-Nicholson VO2+/VO2+ yokuhlola ukusebenza kahle kokusabalalisa nokuthola amanani we-k0(d).
Akukhona nje kuphela ukuthi i-HWO-50% C76 yayibonisa cishe umsebenzi ofanayo we-electrocatalytic njenge-C76 yokusabela kwe-VO2+/VO2+, kodwa, okuthakazelisa nakakhulu, iphinde yacindezela ukuvela kwe-chlorine uma kuqhathaniswa ne-C76, njengoba kuboniswe ku-Fig.6d (RCT ephansi).I-C76 ibonise i-Ipa/Ipc esobala ephakeme kune-HWO-50% C76 (Ithebula S3), hhayi ngenxa yokuhlehliswa kokusabela okuthuthukisiwe, kodwa ngenxa yokunqwabelanisa okuphezulu kokusabela kokunciphisa i-chlorine ne-SHE ku-1.2 V. Ukusebenza okungcono kakhulu kwe-HWO- I-50% C76 ibalulwe kumphumela ongemuhle we-synergistic kanye ne-C76 esebenzayo ye-synergistic kanye ne-WH-OH ephezulu yokushaja okunegethivu ku-HWO.Ukukhishwa kwe-chlorine encane kuzothuthukisa ukusebenza kahle kokushaja kweseli eligcwele, kuyilapho i-kinetics ethuthukisiwe izothuthukisa ukusebenza kahle kwevoltheji yeseli egcwele.
Ngokusho kwe-equation S1, ekuphenduleni okungahlehliswa kabusha (okuhamba kancane kancane kwe-electron) okulawulwa ukusabalalisa, inani eliphakeme lamanje (IP) lincike enanini lama-electron (n), indawo ye-electrode (A), i-diffusion coefficient (D), inombolo yokudlulisa ama-electron (α) nesivinini sokuskena (ν).Ukuze kufundwe ukuziphatha okulawulwa ukusabalalisa kwezinto ezihloliwe, ubudlelwano phakathi kwe-IP ne-ν1/2 bahlelwa futhi bethulwa ku-Fig. 6b.Njengoba zonke izinto ezisetshenziswayo zibonisa ubudlelwano bomugqa, ukusabela kulawulwa ukusabalalisa.Njengoba impendulo ye-VO2+/VO2+ ikwazi ukuhlehliswa ngendlela efanayo, ukuthambeka komugqa kuncike ku-coefficient yokusabalalisa kanye nenani lika-α (isibalo S1).Njengoba i-diffusion coefficient ingaguquki (≈ 4 × 10–6 cm2/s) 52, umehluko emthambekeni womugqa ubonisa ngokuqondile amanani ahlukene ka-α, ngakho-ke izinga lokudlulisa i-electron endaweni ye-electrode, ekhonjiswa ku-C76 kanye ne-HWO -50% C76 emthambekeni ophakeme kakhulu (isilinganiso sokudlulisa i-electron esiphezulu).
Imithambeka ye-Warburg (W) ibalwe amaza aphansi aboniswe kuThebula S3 (Fig. 6d) inamanani asondele koku-1 kuzo zonke izinto zokwakha, okubonisa ukusakazeka okuphelele kwezinhlobo ze-redox futhi eqinisekisa ukuziphatha okuqondile kwe-IP uma kuqhathaniswa no-ν1/ 2. I-CV iyakalwa.Ku-HWO-50% C76, i-Warburg slope ichezuka isuka ku-1 iye ku-1.32, ikhombisa hhayi kuphela ukusabalalisa okungapheli kwe-reagent (VO2+), kodwa futhi negalelo elingaba khona lokuziphatha kongqimba oluncane ekuziphatheni kokusabalalisa ngenxa ye-electrode porosity.
Ukuze kuqhutshekwe kuhlaziywe ukuhlehla (isilinganiso sokudlulisa ama-electron) sokusabela kwe-VO2+/VO2+ redox, indlela yokusabela ye-Nicholson quasi-reversible reversible nayo yasetshenziswa ukuze kunqunywe izinga elijwayelekile elingu-k041.42.Lokhu kwenziwa kusetshenziswa i-equation ye-S2 ukuze kwakhiwe ipharamitha yekinetic engena dimensionless Ψ, okuwumsebenzi we-ΔEp, njengomsebenzi ka-ν-1/2.Ithebula elithi S4 libonisa amanani angu-Ψ atholakale ku-electrode material ngayinye.Imiphumela (Fig. 6c) yahlelwa ukuze kutholwe u-k0 × 104 cm/s ukusuka emthambekeni wesakhiwo ngasinye kusetshenziswa i-Equation S3 (ebhalwe eduze komugqa ngamunye futhi yethulwe kuThebula S4).I-HWO-50% i-C76 itholakale ine-slope ephakeme kakhulu (Fig. 6c), ngakho-ke inani eliphakeme le-k0 liyi-2.47 × 10-4 cm / s.Lokhu kusho ukuthi le electrode ifinyelela i-kinetics esheshayo, ehambisana nemiphumela ye-CV ne-EIS ku-Fig. 6a no-d nakuThebula S3.Ukwengeza, inani le-k0 liphinde latholakala ku-Nyquist plot (Fig. 6d) ye-Equation S4 kusetshenziswa inani le-RCT (Ithebula S3).Le miphumela ye-k0 evela ku-EIS ifingqwe kuThebula S4 futhi iphinde ibonise ukuthi i-HWO-50% C76 ibonisa izinga eliphezulu lokudlulisa ama-electron ngenxa yomphumela we-synergistic.Noma amanani e-k0 ehluka ngenxa yemvelaphi ehlukene yendlela ngayinye, asabonisa ukuhleleka okufanayo kobukhulu futhi abonise ukungaguquguquki.
Ukuze uqonde ngokugcwele ama-kinetics amahle kakhulu atholiwe, kubalulekile ukuqhathanisa izinto ezifanele ze-electrode nama-electrode e-UCC angavaliwe kanye ne-TCC.Ekuphenduleni kwe-VO2+/VO2+, i-HWO-C76 ayizange ibonise kuphela i-ΔEp ephansi kakhulu kanye nokuhlehla okungcono, kodwa futhi yacindezela kakhulu ukusabela kokuvela kwe-chlorine eyisinambuzane uma kuqhathaniswa ne-TCC, njengoba kukalwa okwamanje ku-1.45 V uma kuqhathaniswa ne-SHE (Fig. 7a).Mayelana nokuzinza, sicabange ukuthi i-HWO-50% C76 yayizinzile ngokomzimba ngoba i-catalyst yayixubene ne-PVDF binder bese isetshenziswa kuma-electrode endwangu ye-carbon.I-HWO-50% C76 ibonise ukushintsha okuphezulu kwe-44 mV (izinga lokuwohloka kwe-0.29 mV/umjikelezo) ngemva kwemijikelezo engu-150 uma kuqhathaniswa ne-50 mV ye-UCC (Umfanekiso 7b).Lokhu kungase kungabi umehluko omkhulu, kodwa i-kinetics yama-electrode e-UCC ihamba kancane futhi yehlisa isithunzi uma uhamba ngebhayisikili, ikakhulukazi ukusabela okuhlanekezelwe.Nakuba ukubuyiselwa emuva kwe-TCC kungcono kakhulu kunaleyo ye-UCC, i-TCC itholwe inokushintsha okukhulu kwe-73 mV ngemva kwemijikelezo engu-150, okungenzeka kube ngenxa yenani elikhulu le-chlorine elakhiwe phezu kwayo.ukuze i-catalyst ibambelele kahle endaweni ye-electrode.Njengoba kungabonakala kuwo wonke ama-electrode ahloliwe, ngisho nama-electrode angenawo ama-catalyst asekelwe abonise amazinga ahlukene okungazinzi kokuhamba ngebhayisikili, okuphakamisa ukuthi ukuguqulwa kokuhlukana okuphezulu ngesikhathi sokuhamba ngebhayisikili kungenxa yokuvalwa kwento ebangelwa izinguquko zamakhemikhali kunokuhlukana kwe-catalyst.Ukwengeza, uma inani elikhulu lezinhlayiya ze-catalyst lizohlukaniswa ebusweni be-electrode, lokhu kuzoholela ekwandeni okuphawulekayo kokuhlukaniswa okuphezulu (hhayi kuphela i-44 mV), njengoba i-substrate (UCC) ingasebenzi ngokuqhathaniswa ne-VO2 +/VO2+ redox reaction.
Ukuqhathaniswa kwe-CV yezinto ezingcono kakhulu ze-electrode uma kuqhathaniswa ne-UCC (a) nokuzinza kwe-VO2+/VO2+ redox reaction (b).ν = 5 mV/s kuwo wonke ama-CV ku-0.1 M VOSO4/1 M H2SO4 + 1 M HCl electrolyte.
Ukwandisa ukukhanga kwezomnotho kobuchwepheshe be-VRFB, ukwandisa nokuqonda i-kinetics yokusabela kwe-vanadium redox kubalulekile ukuze kuzuzwe ukusebenza kahle kwamandla okuphezulu.Izinhlanganisela ze-HWO-C76 zalungiswa futhi umphumela wazo we-electrocatalytic ekuphenduleni kwe-VO2+/VO2+ wacwaningwa.I-HWO ibonise ukuthuthukiswa okuncane kwe-kinetic kuma-electrolyte ane-asidi exubile kodwa yacindezela kakhulu ukuvela kwe-chlorine.Izilinganiso ezihlukahlukene ze-HWO:C76 zisetshenzisiwe ukuze kuthuthukiswe i-kinetics yama-electrode asekelwe ku-HWO.Ukwenyuka kwe-C76 kuya ku-HWO kuthuthukisa i-electron transfer kinetics ye-VO2+/VO2+ reaction on the modified electrode, lapho i-HWO-50% C76 iyimpahla engcono kakhulu ngoba yehlisa ukumelana nokushajwa futhi icindezela ngokwengeziwe i-chlorine uma iqhathaniswa ne-C76 nediphozi ye-TCC..Lokhu kungenxa yomphumela we-synergistic phakathi kwe-C=C sp2 hybridization, i-OH kanye namaqembu asebenzayo e-W-OH.Izinga lokuwohloka ngemva kokuhamba ngebhayisikili okuphindaphindiwe kwe-HWO-50% C76 litholakale liyi-0.29 mV/umjikelezo, kuyilapho izinga lokuwohloka kwe-UCC ne-TCC lingu-0.33 mV/umjikelezo kanye no-0.49 mV/umjikelezo, ngokulandelana, okwenza izinze kakhulu.kuma-electrolyte e-asidi ehlanganisiwe.Imiphumela ethulwe ihlonze ngempumelelo izinto zokwenziwa kwama-electrode ezisezingeni eliphezulu zokusabela kwe-VO2+/VO2+ nge-kinetics esheshayo nokuzinza okuphezulu.Lokhu kuzonyusa amandla kagesi okukhiphayo, ngaleyo ndlela kwandise ukusebenza kahle kwamandla kwe-VRFB, ngaleyo ndlela kunciphise izindleko zokudayiswa kwayo esikhathini esizayo.
Amasethi edatha asetshenzisiwe kanye/noma ahlaziywa ocwaningweni lwamanje ayatholakala kubabhali abafanele uma kunesicelo esifanele.
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