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Izindleko eziphakeme kakhulu zamabhethri e-all-vanadium flow-through redox (ama-VRFB) zinciphisa ukusetshenziswa kwawo kabanzi. Ukuthuthukisa i-kinetics ye-electrochemical reactions kuyadingeka ukwandisa amandla athile kanye nokusebenza kahle kwamandla kwe-VRFB, ngaleyo ndlela kunciphisa izindleko ze-kWh ze-VRFB. Kulo msebenzi, ama-nanoparticles e-tungsten oxide (HWO) ahlanganiswe ngamanzi, i-C76 kanye ne-C76/HWO, afakwe kuma-electrode endwangu yekhabhoni futhi ahlolwa njenge-electrocatalysts ye-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 Fourier transform Spectroscopy (FTIR) kanye nokulinganiswa kwe-contact angle. Kutholakale ukuthi ukungezwa kwama-fullerenes e-C76 ku-HWO kungathuthukisa i-electrode kinetics ngokwandisa ukuhanjiswa kukagesi kanye nokuhlinzeka ngamaqembu okusebenza a-oxidized ebusweni bawo, ngaleyo ndlela kukhuthaze ukusabela kwe-VO2+/VO2+ redox. I-HWO/C76 composite (50 wt% C76) ibonakale iyisinqumo esingcono kakhulu sokusabela kwe-VO2+/VO2+ nge-ΔEp ye-176 mV, kuyilapho indwangu yekhabhoni engalashwanga (UCC) yayingu-365 mV. Ngaphezu kwalokho, i-HWO/C76 composite ibonise umphumela obalulekile wokuvimbela ekusabeleni kokuvela kwe-chlorine okubangelwa yiqembu elisebenzayo le-W-OH.
Umsebenzi omkhulu wabantu kanye noguquko olusheshayo lwezimboni kuholele ekudingweni okukhulu kukagesi okunganqandeki, okwanda cishe ngo-3% ngonyaka1. Sekungamashumi eminyaka, ukusetshenziswa kabanzi kwamafutha emvelo njengomthombo wamandla kuholele ekukhishweni kwamagesi okushisa okufaka isandla ekufudumaleni komhlaba, ukungcola kwamanzi nomoya, okusongela yonke imvelo. Ngenxa yalokho, ukungena kwamandla omoya ahlanzekile navuselelekayo kanye nelanga kulindeleke ukuthi kufinyelele ku-75% kagesi ophelele ngo-20501. Kodwa-ke, lapho isabelo sikagesi esivela emithonjeni evuselelekayo sidlula u-20% wokukhiqiza ugesi okuphelele, igridi iba engazinzile.
Phakathi kwazo zonke izinhlelo zokugcina amandla njengebhethri lokugeleza kwe-vanadium redox elihlanganisiwe2, ibhethri lokugeleza kwe-all-vanadium redox (VRFB) lithuthuke ngokushesha kakhulu ngenxa yezinzuzo zalo eziningi futhi libhekwa njengesixazululo esingcono kakhulu sokugcina amandla isikhathi eside (cishe iminyaka engama-30). ) Izinketho ezihlanganiswe namandla avuselelekayo4. Lokhu kungenxa yokuhlukaniswa kwamandla namandla, impendulo esheshayo, impilo yesevisi ende, kanye nezindleko eziphansi zonyaka ezingama-$65/kWh uma kuqhathaniswa namabhethri e-Li-ion nama-lead-acid angama-$93-140/kWh kanye namadola ase-US angama-279-420 nge-kWh. 4.
Kodwa-ke, ukuthengiswa kwazo okukhulu kusavinjelwe yizindleko zazo ezinkulu zesistimu, ikakhulukazi ngenxa yama-cell stacks4,5. Ngakho-ke, ukuthuthukisa ukusebenza kwe-stack ngokwandisa i-kinetics ye-half-element reactions ezimbili kunganciphisa usayizi we-stack ngaleyo ndlela kunciphise izindleko. Ngakho-ke, ukudluliselwa okusheshayo kwe-electron ebusweni be-electrode kuyadingeka, okuncike ekuklanyweni, ukwakheka kanye nesakhiwo se-electrode futhi kudinga ukulungiswa ngokucophelela6. Naphezu kokuzinza okuhle kwamakhemikhali kanye ne-electrochemical kanye nokuqhuba kahle kukagesi kwama-carbon electrodes, i-kinetics yazo engalashwanga iyahamba kancane ngenxa yokungabikho kwamaqembu asebenzayo e-oxygen kanye ne-hydrophilicity7,8. Ngakho-ke, ama-electrocatalyst ahlukahlukene ahlanganiswa nama-electrode asekelwe ku-carbon, ikakhulukazi ama-carbon nanostructures kanye nama-metal oxides, ukuthuthukisa i-kinetics yawo womabili ama-electrode, ngaleyo ndlela kwandiswe i-kinetics ye-VRFB electrode.
Ngaphezu komsebenzi wethu wangaphambilini ku-C76, siqale sabika umsebenzi omuhle kakhulu we-electrocatalytic waleli fullerene we-VO2+/VO2+, ukudluliswa kweshaja, uma kuqhathaniswa nendwangu yekhabhoni ephathwe ngokushisa nengaphathwanga. Ukumelana kuncishiswe ngo-99.5% kanye no-97%. Ukusebenza kwe-catalytic kwezinto zekhabhoni zokusabela kwe-VO2+/VO2+ uma kuqhathaniswa ne-C76 kuboniswe kuThebula S1. Ngakolunye uhlangothi, ama-oxide amaningi ensimbi njenge-CeO225, ZrO226, MoO327, NiO28, SnO229, Cr2O330 kanye ne-WO331, 32, 33, 34, 35, 36, 37 asetshenziswe ngenxa yokumanzi kwawo okwandisiwe kanye nokusebenza kwe-oxygen eningi. , 38. iqembu. Umsebenzi we-catalytic walezi oxide zensimbi ku-reaction ye-VO2+/VO2+ uvezwe kuThebula S2. I-WO3 isetshenziswe emisebenzini eminingi ngenxa yezindleko zayo eziphansi, ukuzinza okuphezulu kwe-acidic media, kanye nomsebenzi ophezulu we-catalytic31,32,33,34,35,36,37,38. Kodwa-ke, ukuthuthuka kwe-cathodic kinetics ngenxa ye-WO3 akubalulekile. Ukuze kuthuthukiswe ukuhanjiswa kwe-WO3, umphumela wokusebenzisa i-tungsten oxide encishisiwe (W18O49) emsebenzini we-cathodic wahlolwa38. I-tungsten oxide emanzi (HWO) ayikaze ihlolwe kuzinhlelo zokusebenza ze-VRFB, yize ikhombisa umsebenzi owandisiwe kuzinhlelo zokusebenza ze-supercapacitor ngenxa yokusabalala kwe-cation okusheshayo uma kuqhathaniswa ne-WOx39,40 engamanzi. Ibhethri lokugeleza kwe-vanadium redox yesizukulwane sesithathu isebenzisa i-electrolyte exubile ye-acid eyakhiwe yi-HCl ne-H2SO4 ukuthuthukisa ukusebenza kwebhethri nokuthuthukisa ukuncibilika kanye nokuqina kwama-ion e-vanadium ku-electrolyte. Kodwa-ke, ukusabela kokuziphendukela kwe-chlorine okubangelwa yizinambuzane sekungenye yezinto ezimbi zesizukulwane sesithathu, ngakho-ke ukufuna izindlela zokuvimbela ukusabela kokuhlolwa kwe-chlorine sekuyinto ebalulekile emaqenjini amaningana ocwaningo.
Lapha, kwenziwa ukuhlolwa kokusabela kwe-VO2+/VO2+ kuma-composite e-HWO/C76 afakwe kuma-electrode endwangu yekhabhoni ukuze kutholakale ibhalansi phakathi kokuqhuba kukagesi kwama-composite kanye ne-redox kinetics ebusweni be-electrode ngenkathi kucindezela impendulo ye-parasitic chlorine evolution. (CER). Ama-nanoparticles e-tungsten oxide (HWO) afakwe ngamanzi ahlanganiswe ngendlela elula ye-hydrothermal. Ukuhlolwa kwenziwa ku-electrolyte exubile ye-acid (H2SO4/HCl) ukuze kulingiswe i-VRFB yesizukulwane sesithathu (G3) ukuze kutholakale ukuthi isebenza kanjani futhi kuphenywe umphumela we-HWO ekusabela 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), sodium Tungsten oxide dihydrate (Na2WO4, 99%, Sigma-Aldrich) kanye ne-hydrophilic carbon cloth ELAT (Fuel Cell Store) kwasetshenziswa kulolu cwaningo.
I-tungsten oxide (HWO) enamanzi yalungiswa nge-hydrothermal reaction 43 lapho u-2 g wosawoti we-Na2WO4 wancibilikiswa ku-12 ml we-H2O ukuze kunikezwe isisombululo esingenambala, kwabe sekufakwa u-12 ml we-2 M HCl ukuze kunikezwe i-suspension ephuzi elikhanyayo. I-slurry yafakwa ku-autoclave yensimbi engagqwali eboshwe yi-Teflon futhi yagcinwa kuhhavini ku-180° C. amahora ama-3 ukuze kutholakale i-hydrothermal reaction. Izinsalela zaqoqwa ngokuhluzwa, zagezwa izikhathi ezintathu nge-ethanol namanzi, zomiswa kuhhavini ku-70°C amahora angama-3, bese zihluzwa ukuze kunikezwe i-powder ye-HWO eluhlaza okwesibhakabhaka.
Ama-electrode endwangu yekhabhoni atholiwe (angalungiswanga) (CCT) asetshenziswe njengoba enjalo noma aphathwe ngokushisa esithandweni sepayipi ku-450°C emoyeni ngesilinganiso sokushisa esingu-15 ºC/min amahora ayi-10 ukuthola ama-CC aphathwe (TCC). Njengoba kuchaziwe esihlokweni esandulele. 24. I-UCC ne-TCC zanqunywa zaba ama-electrode angaba ngu-1.5 cm ububanzi kanye no-7 cm ubude. Ukumiswa kwe-C76, HWO, HWO-10% C76, HWO-30% C76 kanye ne-HWO-50% C76 kwalungiswa ngokungeza i-20 mg .% (~2.22 mg) ye-PVDF binder ku-~1 ml DMF futhi kwafakwa i-sonication ihora eli-1 ukuthuthukisa ukufana. 2 mg we-C76, HWO kanye ne-HWO-C76 composites zisetshenziswe ngokulandelana endaweni ye-electrode esebenzayo ye-UCC engaba ngu-1.5 cm2. Zonke izikhuthazi zafakwa kuma-electrode e-UCC kanti i-TCC yasetshenziselwa izinjongo zokuqhathanisa kuphela, njengoba umsebenzi wethu wangaphambilini ubonise ukuthi ukwelashwa kokushisa kwakungadingeki. Ukumiswa kombono kwafezwa ngokuxubha i-100 µl yokumiswa (umthwalo ongu-2 mg) ukuze kube nomphumela olinganayo. Ngemuva kwalokho wonke ama-electrode omisiwe kuhhavini ku-60° C. ubusuku bonke. Ama-electrode alinganiswa phambili nangemuva ukuqinisekisa ukulayisha okunembile kwesitoko. Ukuze kube nendawo ethile yejometri (~1.5 cm2) futhi kuvinjelwe ukukhuphuka kwe-vanadium electrolyte ku-electrode ngenxa yomphumela we-capillary, kwafakwa ungqimba oluncane lwe-paraffin phezu kwezinto ezisebenzayo.
I-field emission scanning electron microscopy (FESEM, Zeiss SEM Ultra 60, 5 kV) yasetshenziswa ukubona isimo sendawo ye-HWO. I-spectrometer ye-X-ray ehlakazekayo efakwe i-Feii8SEM (EDX, Zeiss Inc.) yasetshenziswa ukumaka izakhi ze-HWO-50%C76 kuma-electrode e-UCC. I-microscope ye-electron yokudlulisa enesinqumo esiphezulu (HR-TEM, JOEL JEM-2100) esebenza nge-voltage esheshisa engu-200 kV yasetshenziswa ukuthwebula izithombe zezinhlayiya ze-HWO ezinesinqumo esiphezulu kanye namasongo okusabalalisa. Isofthiwe ye-Crystallography Toolbox (CrysTBox) isebenzisa umsebenzi we-ringGUI ukuhlaziya iphethini yokusabalalisa indandatho ye-HWO nokuqhathanisa imiphumela nephethini ye-XRD. Isakhiwo kanye ne-graphitization ye-UCC kanye ne-TCC kuhlaziywe 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 isakhiwo sekristalu kanye nesigaba se-HWO. Isofthiwe ye-PANalytical X'Pert HighScore yasetshenziswa ukufanisa iziqongo ze-HWO namamephu e-tungsten oxide atholakala ku-database45. Imiphumela ye-HWO iqhathaniswe nemiphumela ye-TEM. Ukwakheka kwamakhemikhali kanye nesimo samasampula e-HWO kunqunywe yi-X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi, ThermoScientific). Isofthiwe ye-CASA-XPS (v 2.3.15) yasetshenziselwa ukuhlukanisa i-peak kanye nokuhlaziywa kwedatha. Ukuze kutholakale amaqembu okusebenza ebusweni be-HWO kanye ne-HWO-50%C76, kwenziwa izilinganiso kusetshenziswa i-Fourier transform infrared spectroscopy (FTIR, Perkin Elmer spectrometer, kusetshenziswa i-KBr FTIR). Imiphumela iqhathaniswe nemiphumela ye-XPS. Izilinganiso ze-contact angle (KRUSS DSA25) nazo zasetshenziswa ukuchaza ukumanzi kwama-electrode.
Kuzo zonke izilinganiso ze-electrochemical, kusetshenziswe i-workstation ye-Biologic SP 300. I-cyclic voltammetry (CV) kanye ne-electrochemical impedance spectroscopy (EIS) zasetshenziswa ukutadisha i-electrode kinetics ye-VO2+/VO2+ redox reaction kanye nomphumela we-reagent diffusion (VOSO4(VO2+)) esilinganisweni sokusabela. Zombili izindlela zisebenzise iseli lama-electrode amathathu eline-electrolyte concentration engu-0.1 M VOSO4 (V4+) ku-1 M H2SO4 + 1 M HCl (ingxube yama-asidi). Yonke idatha ye-electrochemical eyethulwe ilungisiwe nge-IR. I-saturated calomel electrode (SCE) kanye ne-platinum (Pt) coil zasetshenziswa njenge-reference kanye ne-counter electrode, ngokulandelana. Ku-CV, amazinga okuskena (ν) angu-5, 20, kanye no-50 mV/s asetshenziswe kufasitela elinamandla le-VO2+/VO2+ le-(0–1) V vs. SCE, bese kulungiselelwa i-SHE ukuze idwebe (VSCE = 0.242 V vs. HSE). Ukuze kufundwe ukugcinwa komsebenzi we-electrode, ama-CV aphindaphindwayo aphindaphindwayo enziwe ku-ν 5 mV/s ye-UCC, TCC, UCC-C76, UCC-HWO, kanye ne-UCC-HWO-50% C76. Ekulinganisweni kwe-EIS, ububanzi bemvamisa yokusabela kwe-redox ye-VO2+/VO2+ babungu-0.01-105 Hz, kanti ukuphazamiseka kwe-voltage ku-voltage ye-open-circuit (OCV) kwakungu-10 mV. Ukuhlolwa ngakunye kwaphindwa izikhathi ezingu-2-3 ukuqinisekisa ukuvumelana kwemiphumela. Ama-variant rate ahlukene (k0) atholwe ngendlela ye-Nicholson46,47.
I-tungsten oxide (HVO) enamanzi ikhiqizwe ngempumelelo ngendlela ye-hydrothermal. Isithombe se-SEM ku-fig. 1a sibonisa ukuthi i-HWO efakiwe iqukethe amaqoqo e-nanoparticles anobukhulu obuphakathi kuka-25-50 nm.
Iphethini ye-X-ray diffraction ye-HWO ikhombisa iziqongo (001) kanye no-(002) ku-~23.5° kanye no-~47.5°, ngokulandelana, okuyizimpawu ze-WO2.63 engeyona i-stoichiometric (W32O84) (PDF 077–0810, a = 21.4 Å, b = 17.8 Å, c = 3.8 Å, α = β = γ = 90°), okuhambisana nombala wazo oluhlaza okwesibhakabhaka ocacile (Isithombe 1b) 48.49. Ezinye iziqongo cishe ku-20.5°, 27.1°, 28.1°, 30.8°, 35.7°, 36.7° kanye no-52.7° zabelwe ku-(140), (620), (350), (720), (740), (560°). ) ) kanye (970) i-diffraction ijikeleza i-orthogonal ku-WO2.63, ngokulandelana. Indlela efanayo yokwenziwa yasetshenziswa nguSongara et al. 43 ukuthola umkhiqizo omhlophe, okwabangelwa ukuba khona kwe-WO3(H2O)0.333. Kodwa-ke, kulo msebenzi, ngenxa yezimo ezahlukene, kwatholakala umkhiqizo oluhlaza okwesibhakabhaka ompunga, okubonisa 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°) kanye nefomu elincishisiwe le-tungsten 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+ kanye ne-W4+ (1.67:1 W6+:W4+), okuqukethwe okulinganiselwe kwe-W6+ kanye ne-W4+ cishe kungama-72% W6+ kanye nama-28% W4+, ngokulandelana. Izithombe ze-SEM, ama-spectra e-XPS angumzuzwana owodwa ezingeni le-nucleus, izithombe ze-TEM, ama-spectra e-FTIR, kanye nama-spectra e-Raman ezinhlayiya ze-C76 zethulwe esihlokweni sethu esedlule. Ngokusho kukaKawada et al., i-50,51 i-X-ray diffraction ye-C76 ngemva kokususwa kwe-toluene ibonise isakhiwo se-monoclinic se-FCC.
Izithombe ze-SEM ku-fig. 2a kanye no-b zibonisa ukuthi i-HWO kanye ne-HWO-50%C76 zifakwe ngempumelelo kuma-carbon fibers e-UCC electrode naphakathi kwawo. Amamephu e-EDX element e-tungsten, i-carbon, kanye ne-oxygen ezithombeni ze-SEM ku-fig. 2c aboniswe ku-fig. 2d-f okubonisa ukuthi i-tungsten ne-carbon kuxutshwe ngokulinganayo (kubonisa ukusatshalaliswa okufanayo) phezu kobuso bonke be-electrode futhi i-composite ayifakwanga ngokulinganayo ngenxa yemvelo yendlela yokufaka.
Izithombe ze-SEM zezinhlayiya ze-HWO ezifakiwe (a) kanye nezinhlayiya ze-HWO-C76 (b). Imephu ye-EDX ku-HWO-C76 elayishwe ku-UCC kusetshenziswa indawo esesithombeni (c) ikhombisa ukusatshalaliswa kwe-tungsten (d), i-carbon (e), kanye ne-oxygen (f) kusampula.
I-HR-TEM yasetshenziselwa ukuthwebula izithombe zokukhulisa okuphezulu kanye nolwazi lwekristalografi (Isithombe 3). I-HWO ikhombisa ukuma kwe-nanocube njengoba kuboniswe ku-Fig. 3a futhi kucace kakhudlwana ku-Fig. 3b. Ngokukhulisa i-nanocube ukuze kuhlukaniswe izindawo ezikhethiwe, umuntu angabona ngeso lengqondo isakhiwo se-grating kanye nezindiza ze-diffraction ezihlangabezana nomthetho we-Bragg, njengoba kuboniswe ku-Fig. 3c, okuqinisekisa ubukristali bezinto ezibonakalayo. Esihlokweni esingezansi ku-Fig. 3c sibonisa ibanga d 3.3 Å elihambisana nezindiza ze-diffraction (022) kanye (620) ezitholakala ezigabeni ze-WO3(H2O)0.333 kanye ne-W32O84, ngokulandelana43,44,49. Lokhu kuhambisana nokuhlaziywa kwe-XRD okuchazwe ngenhla (Isithombe 1b) njengoba ibanga lendiza ye-grating elibonwe d (Isithombe 3c) lihambisana ne-XRD peak enamandla kakhulu kusampula ye-HWO. Amasongo esampula nawo aboniswe ku-Fig. 3d, lapho indandatho ngayinye ihambelana nendiza ehlukile. Izindiza ze-WO3(H2O)0.333 kanye ne-W32O84 zinombala omhlophe noluhlaza okwesibhakabhaka, ngokulandelana, futhi iziqongo zazo ze-XRD ezifanayo nazo ziboniswe ku-Fig. 1b. Indandatho yokuqala eboniswe kumdwebo wendandatho ihambelana nenhloko yokuqala ephawulwe kuphethini ye-x-ray yendiza ye-diffraction (022) noma (620). Kusukela emasongweni (022) kuya ku-(402), amanani e-d-spacing angu-3.30, 3.17, 2.38, 1.93, kanye no-1.69 Å, ahambisana 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 esikhulisiwe. Izithombe zezindiza ezigobile ziboniswe ku-(c), isithombe esingaphakathi (c) sibonisa isithombe esikhulisiwe sezindiza kanye nephimbo d elingu-0.33 nm elihambisana nezindiza (002) kanye ne-(620). (d) Iphethini yendandatho ye-HWO ekhombisa izindiza ezihlotshaniswa ne-WO3(H2O)0.333 (emhlophe) kanye ne-W32O84 (eluhlaza okwesibhakabhaka).
Ukuhlaziywa kwe-XPS kwenziwe ukuze kutholakale i-surface chemistry kanye nesimo se-oxidation se-tungsten (Izithombe S1 kanye no-4). Ububanzi be-XPS scan spectrum ye-HWO eyenziwe buboniswe ku-Figure S1, okubonisa ukuba khona kwe-tungsten. Ama-XPS narrow-scan spectra amazinga ayinhloko e-W 4f kanye ne-O 1s aboniswe ku-Figs. 4a kanye no-b, ngokulandelana. I-W 4f spectrum ihlukana ibe ama-doublet amabili e-spin-orbit ahambisana namandla okubopha e-W oxidation state. kanye ne-W 4f7/2 ku-36.6 kanye ne-34.9 eV ayisici se-W4+ state esingu-40, ngokulandelana. )0.333. Idatha efakiwe ikhombisa ukuthi amaphesenti e-athomu e-W6+ kanye ne-W4+ angama-85% kanye no-15%, ngokulandelana, asondele kumanani alinganiswe kudatha ye-XRD uma kucatshangelwa umehluko phakathi kwezindlela ezimbili. Zombili izindlela zinikeza ulwazi oluningi ngokunemba okuphansi, ikakhulukazi i-XRD. Futhi, lezi zindlela ezimbili zihlaziya izingxenye ezahlukene zezinto ngoba i-XRD iyindlela yobuningi kuyilapho i-XPS iyindlela yobuso esondela kuma-nanometer ambalwa kuphela. I-spectrum ye-O1s ihlukaniswe ngama-peaks amabili ku-533 (22.2%) kanye no-530.4 eV (77.8%). Eyokuqala ihambelana ne-OH, kanti eyesibili ihambisana nezibopho ze-oxygen ku-lattice ku-WO. Ukuba khona kwamaqembu asebenzayo e-OH kuhambisana nezakhiwo ze-hydration ze-HWO.
Ukuhlaziywa kwe-FTIR kwenziwe nakulezi zibonelo ezimbili ukuhlola ukuba khona kwamaqembu asebenzayo kanye nama-molecule amanzi axhumanisayo esakhiweni se-HWO esimanzi. Imiphumela ikhombisa ukuthi isampula ye-HWO-50% C76 kanye nemiphumela ye-FT-IR HWO ibonakala ifana ngenxa yokuba khona kwe-HWO, kodwa ukuqina kweziqongo kuyahluka ngenxa yenani elihlukile lesampula elisetshenziswe ukulungiselela ukuhlaziywa (Isithombe 5a). ) I-HWO-50% C76 ikhombisa ukuthi zonke iziqongo, ngaphandle kwesiqongo se-tungsten oxide, zihlobene ne-fullerene 24. Imininingwane eningiliziwe ku-Fig. 5a ikhombisa ukuthi womabili amasampula abonisa ibhendi ebanzi enamandla kakhulu ku-~710/cm ebangelwa ukushukuma kwe-OWO esakhiweni se-lattice se-HWO, enehlombe eliqinile ku-~840/cm ebangelwa yi-WO. Ekushukumeni kokunwebeka, ibhendi ebukhali cishe ku-1610/cm ibangelwa ukugoba kokudlidliza kwe-OH, kuyilapho ibhendi yokumunca ebanzi cishe ku-3400/cm ibangelwa ukudlidliza kwe-OH emaqenjini e-hydroxyl43. Le miphumela ihambisana nama-spectra e-XPS ku-Figs. 4b, lapho amaqembu asebenzayo e-WO anganikeza khona amasayithi asebenzayo okusabela kwe-VO2+/VO2+.
Ukuhlaziywa kwe-FTIR kwe-HWO kanye ne-HWO-50% C76 (a), kuboniswe amaqembu asebenzayo kanye nokulinganiswa kwe-contact angle (b, c).
Iqembu le-OH lingaphinde likhuthaze ukusabela kwe-VO2+/VO2+, ngenkathi kukhulisa i-hydrophilicity ye-electrode, ngaleyo ndlela kukhuthazwe izinga lokusabalala kanye nokudluliswa kwama-electron. Njengoba kubonisiwe, isampula ye-HWO-50% C76 ikhombisa i-peak eyengeziwe ye-C76. Iziqongo ku-~2905, 2375, 1705, 1607, kanye ne-1445 cm3 zingabelwa ku-CH, O=C=O, C=O, C=C, kanye nokudlidliza kwe-CO, ngokulandelana. Kwaziwa kahle ukuthi amaqembu asebenzayo e-oxygen C=O kanye ne-CO angasebenza njengezikhungo ezisebenzayo zokusabela kwe-redox kwe-vanadium. Ukuhlola nokuqhathanisa ukumanzi kwama-electrode amabili, kuthathwe izilinganiso ze-contact angle njengoba kuboniswe ku-Fig. 5b,c. I-HWO electrode yamunca amaconsi amanzi ngokushesha, okubonisa i-superhydrophilicity ngenxa yamaqembu asebenzayo e-OH atholakalayo. I-HWO-50% C76 i-hydrophobic kakhulu, ene-contact angle engaba ngu-135° ngemva kwemizuzwana eyi-10. Kodwa-ke, ekulinganisweni kwe-electrochemical, i-electrode ye-HWO-50%C76 yaba manzi ngokuphelele esikhathini esingaphansi komzuzu. Ukulinganiswa kokumanzi kuyahambisana nemiphumela ye-XPS ne-FTIR, okubonisa ukuthi amaqembu amaningi e-OH ebusweni be-HWO enza kube lula kakhulu ukuwa amanzi.
Ukusabela kwe-VO2+/VO2+ kwama-nanocomposites e-HWO kanye ne-HWO-C76 kwahlolwa futhi kwakulindeleke ukuthi i-HWO izocindezela ukuvela kwe-chlorine ku-reaction ye-VO2+/VO2+ ku-acid exubile, kanti i-C76 izoqhubeka nokukhuthaza ukusabela kwe-VO2+/VO2+ redox okufiswayo. %, 30%, kanye no-50% C76 kuma-suspension e-HWO kanye ne-CCC ebekwe kuma-electrode anomthwalo ophelele ongaba ngu-2 mg/cm2.
Njengoba kuboniswe ku-Fig. 6, i-kinetics yokusabela kwe-VO2+/VO2+ ebusweni be-electrode ihlolwe yi-CV ku-electrolyte exubile ye-acid. Ama-currents aboniswa njenge-I/Ipa ukuze kuqhathaniswe kalula i-ΔEp ne-Ipa/Ipc yama-catalysts ahlukene ngqo kugrafu. Idatha yendawo yamanje iboniswe ku-Fig. 2S. Ku-Fig. 6a ikhombisa ukuthi i-HWO ikhulisa kancane izinga lokudluliselwa kwama-electron lokusabela kwe-VO2+/VO2+ redox ebusweni be-electrode futhi icindezela ukusabela kokuvela kwe-chlorine okubangelwa yi-parasitic. Kodwa-ke, i-C76 ikhulisa kakhulu izinga lokudluliselwa kwama-electron futhi ivuselela ukusabela kokuvela kwe-chlorine. Ngakho-ke, inhlanganisela eyenziwe kahle ye-HWO ne-C76 kulindeleke ukuthi ibe nomsebenzi omuhle kakhulu kanye nekhono elikhulu lokuvimbela ukusabela kokuvela kwe-chlorine. Kutholakale ukuthi ngemuva kokwandisa okuqukethwe kwe-C76, umsebenzi we-electrochemical wama-electrode uthuthukile, njengoba kufakazelwa ukwehla kwe-ΔEp kanye nokwanda kwesilinganiso se-Ipa/Ipc (Ithebula S3). Lokhu kuqinisekiswe futhi ngamanani e-RCT akhishwe ku-Nyquist plot ku-Fig. 6d (Ithebula S3), atholakale ehla ngokuqukethwe kwe-C76 okwandayo. Le miphumela ihambisana nocwaningo lukaLi, lapho ukungezwa kwe-mesoporous carbon ku-mesoporous WO3 kubonise i-kinetics yokudluliselwa kweshaja ethuthukisiwe ku-VO2+/VO2+35. Lokhu kubonisa ukuthi ukusabela okuqondile kungancika kakhulu ekuqhutshweni kwe-electrode (C=C bond) 18, 24, 35, 36, 37. Lokhu kungase futhi kube ngenxa yoshintsho ku-geometry yokuxhumana phakathi kwe-[VO(H2O)5]2+ kanye ne-[VO2(H2O)4]+, i-C76 inciphisa i-reaction overvoltage ngokunciphisa amandla ezicubu. Kodwa-ke, lokhu kungenzeka kungenzeki ngama-electrode e-HWO.
(a) Ukuziphatha kwe-cyclic voltammetric (ν = 5 mV/s) kokusabela kwe-VO2+/VO2+ kwe-UCC kanye ne-HWO-C76 composites enezilinganiso ezahlukene ze-HWO:C76 ku-0.1 M VOSO4/1 M H2SO4 + 1 M HCl electrolyte. (b) Indlela ye-Randles-Sevchik kanye (c) nendlela ye-Nicholson VO2+/VO2+ yokuhlola ukusebenza kahle kokusabalalisa nokuthola amanani e-k0(d).
Akukhona nje kuphela ukuthi i-HWO-50% C76 yayibonisa cishe umsebenzi ofanayo we-electrocatalytic njenge-C76 yokusabela kwe-VO2+/VO2+, kodwa, okuthakazelisayo nakakhulu, yacindezela nokuvela kwe-chlorine uma kuqhathaniswa ne-C76, njengoba kuboniswe ku-Fig. 6a, futhi ikhombisa i-Smaller Semicircle ku-fig. 6d (i-RCT ephansi). I-C76 ibonise i-Ipa/Ipc ebonakalayo ephezulu kune-HWO-50% C76 (Ithebula S3), hhayi ngenxa yokuguquguquka kokusabela okuthuthukisiwe, kodwa ngenxa yokuhlangana okuphezulu kokusabela kokunciphisa i-chlorine ne-SHE ku-1.2 V. Ukusebenza okuhle kakhulu kwe-HWO- I-50% C76 ibangelwa umphumela wokubambisana phakathi kwe-C76 ekhokhiswa kabi kanye nokumanzi okuphezulu kanye nokusebenza kwe-W-OH catalytic ku-HWO. Ukukhishwa okuncane kwe-chlorine kuzothuthukisa ukusebenza kahle kokushaja kweseli eligcwele, kuyilapho i-kinetics ethuthukisiwe izothuthukisa ukusebenza kahle kwe-voltage yeseli eligcwele.
Ngokusho kwe-equation S1, ngokusabela okungaguquki (ukudluliselwa kwama-electron kancane) okulawulwa ukusabalala, ugesi ophezulu (IP) uncike enanini lama-electron (n), indawo ye-electrode (A), i-diffusion coefficient (D), inani le-electron transfer coefficient (α) kanye nesivinini sokuskena (ν). Ukuze kufundwe ukuziphatha okulawulwa ukusabalala kwezinto ezivivinyiwe, ubudlelwano phakathi kwe-IP ne-ν1/2 budwetshwe futhi bethulwe ku-Fig. 6b. Njengoba zonke izinto zibonisa ubudlelwano obuqondile, ukusabela kulawulwa ukusabalala. Njengoba ukusabela kwe-VO2+/VO2+ kungashintshashintsha, ukuthambekela komugqa kuncike ku-diffusion coefficient kanye nenani le-α (i-equation S1). Njengoba i-diffusion coefficient ingaguquguquki (≈ 4 × 10–6 cm2/s)52, umehluko emthambekeni womugqa ubonisa ngqo amanani ahlukene e-α, ngakho-ke izinga lokudlulisa ama-electron ebusweni be-electrode, eliboniswa ku-C76 kanye ne-HWO -50% C76 Umthambeke ophakeme kakhulu (izinga lokudlulisa ama-electron eliphakeme kakhulu).
Ama-slope aseWarburg (W) abalwe ngama-frequency aphansi aboniswe kuThebula S3 (Isithombe 6d) anamanani aseduze no-1 kuzo zonke izinto, okubonisa ukusabalala okuphelele kwezinhlobo ze-redox futhi okuqinisekisa ukuziphatha okuqondile kwe-IP uma kuqhathaniswa no-ν1/2. I-CV iyalinganiswa. Ku-HWO-50% C76, i-slope yaseWarburg isuka ku-1 iye ku-1.32, okubonisa hhayi kuphela ukusabalala okungapheli kwe-reagent (VO2+), kodwa futhi nomthelela ongaba khona wokuziphatha okunezingqimba ezincane ekuziphatheni kokusabalala ngenxa ye-electrode porosity.
Ukuze kuhlaziywe kabanzi ukuguquguquka (izinga lokudlulisa i-electron) kwe-VO2+/VO2+ redox reaction, indlela ye-Nicholson quasi-reversible reaction nayo yasetshenziswa ukunquma i-standard rate constant k041.42. Lokhu kwenziwa kusetshenziswa i-S2 equation ukwakha ipharamitha ye-kinetic engenakulinganiswa i-Ψ, okuwumsebenzi we-ΔEp, njengomsebenzi we-ν-1/2. Ithebula i-S4 likhombisa amanani e-Ψ atholakale ezintweni ze-electrode ngayinye. Imiphumela (Isithombe 6c) yadwetshwa ukuze kutholakale i-k0 × 104 cm/s ukusuka emthambekeni we-plot ngayinye kusetshenziswa i-Equation S3 (ebhalwe eceleni komugqa ngamunye futhi yethulwe kuThebula S4). I-HWO-50% C76 itholakale inomthambeke ophezulu kakhulu (Isithombe 6c), ngakho-ke inani eliphakeme kakhulu le-k0 lingu-2.47 × 10–4 cm/s. Lokhu kusho ukuthi le electrode ifinyelela i-kinetics esheshayo, ehambisana nemiphumela ye-CV kanye ne-EIS ku-Fig. 6a kanye no-d kanye naku-Table S3. Ngaphezu kwalokho, inani le-k0 liphinde latholakala ku-Nyquist plot (Fig. 6d) ye-Equation S4 kusetshenziswa inani le-RCT (Table S3). Le miphumela ye-k0 evela ku-EIS ifingqiwe ku-Table S4 futhi ikhombisa nokuthi i-HWO-50% C76 ikhombisa izinga eliphezulu kakhulu lokudlulisa ama-electron ngenxa yomphumela we-synergistic. Ngisho noma amanani e-k0 ehluka ngenxa yemvelaphi ehlukene yendlela ngayinye, asabonisa ukuhleleka okufanayo kobukhulu futhi abonisa ukuvumelana.
Ukuze uqonde ngokugcwele i-kinetics enhle kakhulu etholakele, kubalulekile ukuqhathanisa izinto ze-electrode ezifanele kakhulu nama-electrode e-UCC ne-TCC angagqokwanga. Ngokusabela kwe-VO2+/VO2+, i-HWO-C76 ayizange ibonise kuphela i-ΔEp ephansi kakhulu kanye nokuguqulwa okungcono, kodwa futhi yacindezela kakhulu ukusabela kokuvela kwe-chlorine okubangelwa yi-parasitic uma kuqhathaniswa ne-TCC, njengoba kulinganiswa ngogesi ku-1.45 V uma kuqhathaniswa ne-SHE (Isithombe 7a). Ngokuphathelene nokuzinza, sicabange ukuthi i-HWO-50% C76 yayizinzile ngokomzimba ngoba i-catalyst yaxutshwa ne-PVDF binder yabe isisetshenziswa kuma-electrode endwangu yekhabhoni. I-HWO-50% C76 ibonise ukushintsha okuphezulu kwe-44 mV (izinga lokubola lingu-0.29 mV/umjikelezo) ngemuva kwemijikelezo engu-150 uma kuqhathaniswa ne-50 mV ye-UCC (Isithombe 7b). Lokhu kungase kungabi umehluko omkhulu, kodwa i-kinetics yama-electrode e-UCC ihamba kancane kakhulu futhi iyonakala ngokujikeleza, ikakhulukazi ekuphenduleni okuphambene. Nakuba ukuguqulwa kwe-TCC kungcono kakhulu kunokwe-UCC, i-TCC itholakale inokushintsha okukhulu kwe-peak okungu-73 mV ngemva kwemijikelezo engu-150, okungase kube ngenxa yenani elikhulu le-chlorine elakhiwe ebusweni bayo. ukuze i-catalyst inamathele kahle ebusweni be-electrode. Njengoba kungabonakala kuwo wonke ama-electrode ahlolwe, ngisho nama-electrode angenazo izi-catalyst ezisekelwayo abonise amazinga ahlukahlukene okungazinzi kokujikeleza, okuphakamisa ukuthi ushintsho ekuhlukanisweni kwe-peak ngesikhathi sokujikeleza lubangelwa ukungasebenzi kwezinto ezibangelwa izinguquko zamakhemikhali kunokuhlukaniswa kwe-catalyst. Ngaphezu kwalokho, uma inani elikhulu lezinhlayiya ze-catalyst belingahlukaniswa ebusweni be-electrode, lokhu kuzoholela ekwandeni okukhulu kokuhlukaniswa kwe-peak (hhayi kuphela i-44 mV), njengoba i-substrate (UCC) ingasebenzi kahle ku-VO2+/VO2+ redox reaction.
Ukuqhathaniswa kwe-CV yezinto ezisetshenziswa yi-electrode ezinhle kakhulu uma kuqhathaniswa ne-UCC (a) kanye nokuzinza kokusabela kwe-redox ye-VO2+/VO2+ (b). ν = 5 mV/s kuwo wonke ama-CV ku-0.1 M VOSO4/1 M H2SO4 + 1 M HCl electrolyte.
Ukuze kwandiswe ukukhanga komnotho kobuchwepheshe be-VRFB, ukwandisa nokuqonda i-kinetics ye-vanadium redox reactions kubalulekile ukuze kufezwe ukusebenza kahle kwamandla okuphezulu. Ama-composites HWO-C76 alungiselelwe futhi kwafundwa umphumela wawo we-electrocatalytic ku-VO2+/VO2+ reaction. I-HWO ibonise ukuthuthukiswa okuncane kwe-kinetic kuma-electrolyte axubile acidic kodwa yacindezela kakhulu ukuvela kwe-chlorine. Izilinganiso ezahlukahlukene ze-HWO:C76 zasetshenziswa ukuze kuthuthukiswe i-kinetics yama-electrode asekelwe ku-HWO. Ukwandisa i-C76 ku-HWO kuthuthukisa i-kinetics yokudluliselwa kwama-electrode ye-VO2+/VO2+ reaction ku-electrode eguquliwe, lapho i-HWO-50% C76 iyinto engcono kakhulu ngoba inciphisa ukumelana nokudluliselwa kweshaja futhi icindezela i-chlorine uma kuqhathaniswa ne-C76 kanye ne-TCC deposit. . Lokhu kungenxa yomphumela wokubambisana phakathi kwamaqembu asebenzayo e-C=C sp2 hybridization, i-OH kanye ne-W-OH. Izinga lokuwohloka ngemva kokujikeleza okuphindaphindiwe kwe-HWO-50% C76 kutholakale ukuthi lingu-0.29 mV/umjikelezo, kuyilapho izinga lokuwohloka kwe-UCC kanye ne-TCC lingu-0.33 mV/umjikelezo kanye no-0.49 mV/umjikelezo, ngokulandelana, okwenza kube okuzinzile kakhulu. kuma-electrolyte e-acid axubile. Imiphumela eyethulwe iveza ngempumelelo izinto ze-electrode ezisebenzayo eziphezulu zokusabela kwe-VO2+/VO2+ nge-kinetics esheshayo kanye nokuqina okuphezulu. Lokhu kuzokhulisa i-voltage yokukhipha, ngaleyo ndlela kwandise ukusebenza kahle kwamandla kwe-VRFB, ngaleyo ndlela kuncishiswe izindleko zokuthengiswa kwayo kwesikhathi esizayo.
Amasethi edatha asetshenzisiwe kanye/noma ahlaziywe ocwaningweni lwamanje ayatholakala kubabhali abafanele uma becelwa ngokufanele.
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