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Tus nqi siab ntawm cov roj teeb redox vanadium (VRFBs) txwv tsis pub siv dav. Kev txhim kho kinetics ntawm electrochemical reactions yog qhov yuav tsum tau ua kom lub zog tshwj xeeb thiab kev siv hluav taws xob ntawm VRFB, yog li txo tus nqi ntawm kWh ntawm VRFB. Hauv txoj haujlwm no, hydrothermally synthesized hydrated tungsten oxide (HWO) nanoparticles, C76 thiab C76 / HWO, tau tso rau ntawm cov ntaub carbon electrodes thiab sim ua electrocatalysts rau VO2 + / VO2 + redox reaction. Field emission scanning electron microscopy (FESEM), energy dispersive X-ray spectroscopy (EDX), high-resolution transmission electron microscopy (HR-TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), infrared Fourier transform Spectroscopy (FTIR) thiab kev ntsuas lub kaum sab xis. Nws tau pom tias qhov ntxiv ntawm C76 fullerenes rau HWO tuaj yeem txhim kho electrode kinetics los ntawm kev nce hluav taws xob conductivity thiab muab cov pab pawg oxidized functional rau ntawm nws qhov chaw, yog li txhawb nqa VO2 + / VO2 + redox reaction. Cov HWO / C76 composite (50 wt% C76) tau ua pov thawj tias yog qhov kev xaiv zoo tshaj plaws rau VO2 + / VO2 + reaction nrog ΔEp ntawm 176 mV, thaum cov ntaub carbon tsis kho (UCC) yog 365 mV. Tsis tas li ntawd, cov HWO / C76 composite tau qhia txog kev cuam tshuam tseem ceeb rau cov tshuaj tiv thaiv parasitic chlorine evolution vim yog W-OH functional group.
Kev ua ub ua no ntawm tib neeg thiab kev hloov pauv sai ntawm kev lag luam tau ua rau muaj kev xav tau hluav taws xob ntau heev, uas nce ntxiv li ntawm 3% hauv ib xyoos1. Tau ntau xyoo, kev siv roj av ua lub hauv paus rau lub zog tau ua rau muaj cov pa roj av uas ua rau lub ntiaj teb sov, dej thiab huab cua tsis huv, ua rau muaj kev hem thawj rau tag nrho cov ecosystem. Yog li ntawd, kev nkag mus ntawm cua thiab lub zog hnub ci huv thiab rov ua dua tshiab yuav tsum ncav cuag 75% ntawm tag nrho cov hluav taws xob los ntawm xyoo 20501. Txawm li cas los xij, thaum qhov sib koom ntawm hluav taws xob los ntawm cov chaw rov ua dua tshiab tshaj 20% ntawm tag nrho cov hluav taws xob tsim tawm, lub grid yuav tsis ruaj khov.
Ntawm txhua lub tshuab khaws cia lub zog xws li lub roj teeb hybrid vanadium redox flow2, lub roj teeb all-vanadium redox flow (VRFB) tau tsim kho sai tshaj plaws vim nws muaj ntau yam zoo thiab suav tias yog qhov kev daws teeb meem zoo tshaj plaws rau kev khaws cia lub zog mus sij hawm ntev (kwv yees li 30 xyoo). ) Cov kev xaiv ua ke nrog lub zog rov ua dua tshiab4. Qhov no yog vim muaj kev sib cais ntawm lub zog thiab lub zog ceev, teb sai, lub neej ua haujlwm ntev, thiab tus nqi txhua xyoo qis dua ntawm $ 65 / kWh piv rau $ 93-140 / kWh rau Li-ion thiab lead-acid roj teeb thiab 279-420 US dollars ib kWh. roj teeb feem4.
Txawm li cas los xij, lawv cov lag luam loj tseem raug txwv los ntawm lawv cov nqi peev txheej siab, feem ntau yog vim cov cell stacks4,5. Yog li, kev txhim kho kev ua tau zoo ntawm stack los ntawm kev nce kinetics ntawm ob lub ib nrab-element reactions tuaj yeem txo qhov loj ntawm stack thiab yog li txo tus nqi. Yog li ntawd, kev hloov pauv electron sai mus rau qhov chaw electrode yog qhov tsim nyog, uas nyob ntawm tus qauv tsim, cov khoom sib xyaw thiab cov qauv ntawm electrode thiab xav tau kev ua kom zoo zoo6. Txawm hais tias muaj kev ruaj khov tshuaj lom neeg thiab electrochemical zoo thiab kev ua hluav taws xob zoo ntawm cov electrodes carbon, lawv cov kinetics tsis kho tau qeeb vim tsis muaj cov pab pawg ua haujlwm oxygen thiab hydrophilicity7,8. Yog li ntawd, ntau yam electrocatalysts tau sib xyaw nrog cov electrodes carbon, tshwj xeeb tshaj yog cov carbon nanostructures thiab cov hlau oxides, los txhim kho kinetics ntawm ob qho electrodes, yog li ua rau kinetics ntawm VRFB electrode ntau ntxiv.
Ntxiv rau peb cov haujlwm yav dhau los ntawm C76, peb thawj zaug tshaj tawm txog kev ua haujlwm electrocatalytic zoo heev ntawm cov fullerene no rau VO2 + / VO2 +, kev hloov pauv nqi, piv rau cov ntaub carbon uas tau kho cua sov thiab tsis kho. Kev tsis kam txo qis los ntawm 99.5% thiab 97%. Kev ua haujlwm catalytic ntawm cov ntaub ntawv carbon rau VO2 + / VO2 + tshuaj tiv thaiv piv rau C76 tau pom hauv Rooj S1. Ntawm qhov tod tes, ntau cov hlau oxides xws li CeO225, ZrO226, MoO327, NiO28, SnO229, Cr2O330 thiab WO331, 32, 33, 34, 35, 36, 37 tau siv vim lawv cov dej noo ntau ntxiv thiab muaj ntau cov pa oxygen ua haujlwm. , 38. pawg. Kev ua haujlwm catalytic ntawm cov hlau oxides no hauv VO2 + / VO2 + tshuaj tiv thaiv tau nthuav tawm hauv Rooj S2. WO3 tau siv rau hauv ntau yam haujlwm vim nws tus nqi qis, kev ruaj khov siab hauv cov xov xwm acidic, thiab kev ua haujlwm catalytic siab 31, 32, 33, 34, 35, 36, 37, 38. Txawm li cas los xij, kev txhim kho hauv cathodic kinetics vim WO3 tsis tseem ceeb. Txhawm rau txhim kho qhov conductivity ntawm WO3, qhov cuam tshuam ntawm kev siv txo qis tungsten oxide (W18O49) ntawm kev ua haujlwm cathodic tau sim 38. Hydrated tungsten oxide (HWO) yeej tsis tau sim hauv VRFB daim ntawv thov, txawm hais tias nws qhia txog kev ua haujlwm ntau ntxiv hauv supercapacitor daim ntawv thov vim muaj kev sib kis cation sai dua piv rau anhydrous WOx 39, 40. Lub roj teeb vanadium redox flow tiam thib peb siv cov kua qaub sib xyaw ua ke uas muaj HCl thiab H2SO4 los txhim kho kev ua haujlwm ntawm lub roj teeb thiab txhim kho kev yaj thiab kev ruaj khov ntawm vanadium ions hauv electrolyte. Txawm li cas los xij, cov tshuaj tiv thaiv parasitic chlorine tau dhau los ua ib qho tsis zoo ntawm tiam thib peb, yog li kev tshawb nrhiav txoj hauv kev los tiv thaiv cov tshuaj tiv thaiv chlorine tau dhau los ua qhov tseem ceeb ntawm ntau pawg tshawb fawb.
Ntawm no, VO2+/VO2+ cov kev ntsuam xyuas tshuaj tiv thaiv tau ua tiav rau ntawm HWO/C76 composites uas tso rau ntawm cov ntaub carbon electrodes kom nrhiav tau qhov sib npaug ntawm cov hluav taws xob conductivity ntawm cov composites thiab redox kinetics ntawm qhov chaw electrode thaum tswj hwm cov kab mob parasitic chlorine evolution. teb (CER). Hydrated tungsten oxide (HWO) nanoparticles tau synthesized los ntawm txoj kev hydrothermal yooj yim. Cov kev sim tau ua tiav hauv cov kua qaub sib xyaw (H2SO4/HCl) los simulate tiam thib peb VRFB (G3) rau kev siv tau thiab los tshawb nrhiav qhov cuam tshuam ntawm HWO rau cov kab mob parasitic chlorine evolution reaction.
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) thiab hydrophilic carbon cloth ELAT (Fuel Cell Store) tau siv rau hauv txoj kev tshawb fawb no.
Hydrated tungsten oxide (HWO) tau npaj los ntawm hydrothermal reaction 43 uas 2 g ntawm Na2WO4 ntsev tau yaj rau hauv 12 ml ntawm H2O kom muab cov tshuaj tsis muaj xim, tom qab ntawd 12 ml ntawm 2 M HCl tau ntxiv rau hauv dej kom muab cov kua daj daj. Cov slurry tau muab tso rau hauv Teflon coated stainless hlau autoclave thiab khaws cia rau hauv qhov cub ntawm 180 ° C rau 3 teev rau hydrothermal reaction. Cov seem tau sau los ntawm kev lim dej, ntxuav 3 zaug nrog ethanol thiab dej, ziab hauv qhov cub ntawm 70 ° C rau ~ 3 teev, thiab tom qab ntawd triturated kom muab cov hmoov HWO xiav-grey.
Cov electrodes carbon ntaub (CCT) uas tau txais (tsis tau kho) tau siv raws li nws yog lossis kho cua sov hauv lub cub tawg raj ntawm 450 ° C hauv huab cua nrog tus nqi cua sov ntawm 15 ºC / feeb rau 10 teev kom tau txais CCs kho (TCC). raws li tau piav qhia hauv tsab xov xwm dhau los24. UCC thiab TCC tau txiav rau hauv electrodes kwv yees li 1.5 cm dav thiab 7 cm ntev. Kev ncua ntawm C76, HWO, HWO-10% C76, HWO-30% C76 thiab HWO-50% C76 tau npaj los ntawm kev ntxiv 20 mg .% (~ 2.22 mg) ntawm PVDF binder rau ~ 1 ml DMF thiab sonicated rau 1 teev kom txhim kho kev sib xws. 2 mg ntawm C76, HWO thiab HWO-C76 composites tau siv rau thaj chaw UCC electrode nquag ntawm kwv yees li 1.5 cm2. Txhua cov catalysts tau raug thauj mus rau UCC electrodes thiab TCC tau siv rau kev sib piv xwb, vim peb cov haujlwm yav dhau los qhia tau tias kev kho cua sov tsis tas yuav tsum tau24. Kev daws teeb meem tau ua tiav los ntawm kev txhuam 100 µl ntawm cov tshuaj ncua (thauj 2 mg) rau qhov cuam tshuam ntau dua. Tom qab ntawd tag nrho cov electrodes tau qhuav hauv qhov cub ntawm 60 ° C. ib hmos. Cov electrodes raug ntsuas mus tom ntej thiab rov qab kom ntseeg tau tias muaj qhov chaw thau khoom raug. Yuav kom muaj qee qhov chaw geometric (~ 1.5 cm2) thiab tiv thaiv kev nce ntawm vanadium electrolyte mus rau electrode vim yog cov nyhuv capillary, ib txheej nyias ntawm paraffin tau siv rau saum cov khoom siv nquag.
Siv lub tshuab ntsuas hluav taws xob teb (FESEM, Zeiss SEM Ultra 60, 5 kV) los soj ntsuam qhov morphology ntawm HWO. Siv lub tshuab ntsuas hluav taws xob X-ray uas muaj Feii8SEM (EDX, Zeiss Inc.) los kos duab cov khoom HWO-50%C76 ntawm UCC electrodes. Siv lub tshuab ntsuas hluav taws xob xa hluav taws xob siab (HR-TEM, JOEL JEM-2100) uas ua haujlwm ntawm qhov hluav taws xob nrawm ntawm 200 kV los thaij duab cov khoom me me HWO thiab cov nplhaib diffraction siab dua. Cov software Crystallography Toolbox (CrysTBox) siv lub luag haujlwm ringGUI los tshuaj xyuas tus qauv diffraction HWO thiab piv cov txiaj ntsig nrog tus qauv XRD. Cov qauv thiab graphitization ntawm UCC thiab TCC tau soj ntsuam los ntawm X-ray diffraction (XRD) ntawm tus nqi scan ntawm 2.4 ° / feeb los ntawm 5 ° txog 70 ° nrog Cu Kα (λ = 1.54060 Å) siv Panalytical X-ray diffractometer (Qauv 3600). XRD tau qhia cov qauv siv lead ua thiab theem ntawm HWO. PANalytical X'Pert HighScore software tau siv los phim cov HWO peaks rau cov tungsten oxide maps muaj nyob rau hauv lub database45. HWO cov txiaj ntsig tau piv nrog TEM cov txiaj ntsig. Cov tshuaj lom neeg sib xyaw thiab lub xeev ntawm HWO cov qauv tau txiav txim siab los ntawm X-ray photoelectron spectroscopy (XPS, ESCALAB 250Xi, ThermoScientific). CASA-XPS software (v 2.3.15) tau siv rau qhov siab tshaj plaws deconvolution thiab kev tshuaj xyuas cov ntaub ntawv. Txhawm rau txiav txim siab cov pab pawg ua haujlwm ntawm HWO thiab HWO-50%C76, kev ntsuas tau ua los ntawm kev siv Fourier transform infrared spectroscopy (FTIR, Perkin Elmer spectrometer, siv KBr FTIR). Cov txiaj ntsig tau muab piv rau cov txiaj ntsig XPS. Kev ntsuas lub kaum sab xis (KRUSS DSA25) kuj tau siv los piav qhia txog qhov ntub ntawm cov electrodes.
Rau txhua qhov kev ntsuas electrochemical, Biologic SP 300 workstation tau siv. Cyclic voltammetry (CV) thiab electrochemical impedance spectroscopy (EIS) tau siv los kawm txog electrode kinetics ntawm VO2+/VO2+ redox reaction thiab cov nyhuv ntawm reagent diffusion (VOSO4(VO2+)) ntawm qhov nrawm ntawm kev ua haujlwm. Ob txoj kev siv lub cell peb-electrode nrog qhov electrolyte concentration ntawm 0.1 M VOSO4 (V4+) hauv 1 M H2SO4 + 1 M HCl (sib xyaw ntawm cov kua qaub). Tag nrho cov ntaub ntawv electrochemical uas tau nthuav tawm yog IR kho. Lub electrode calomel saturated (SCE) thiab lub platinum (Pt) coil tau siv ua qhov siv thiab lub electrode counter, raws li. Rau CV, scan rates (ν) ntawm 5, 20, thiab 50 mV/s tau siv rau VO2+/VO2+ lub qhov rais muaj peev xwm rau (0–1) V vs. SCE, tom qab ntawd kho rau SHE kom plot (VSCE = 0.242 V vs. HSE). Txhawm rau kawm txog kev khaws cia ntawm cov electrode activity, rov ua dua cyclic CVs tau ua ntawm ν 5 mV / s rau UCC, TCC, UCC-C76, UCC-HWO, thiab UCC-HWO-50% C76. Rau kev ntsuas EIS, qhov zaus ntawm VO2 + / VO2 + redox reaction yog 0.01-105 Hz, thiab qhov voltage perturbation ntawm qhib-circuit voltage (OCV) yog 10 mV. Txhua qhov kev sim tau rov ua dua 2-3 zaug kom ntseeg tau tias muaj kev sib xws ntawm cov txiaj ntsig. Cov heterogeneous rate constants (k0) tau txais los ntawm Nicholson method46,47.
Hydrated tungsten oxide (HVO) tau raug tsim los ntawm txoj kev hydrothermal. Daim duab SEM hauv daim duab 1a qhia tau hais tias HWO uas tau tso tawm muaj cov pawg ntawm cov nanoparticles nrog qhov loj me ntawm 25-50 nm.
Tus qauv X-ray diffraction ntawm HWO qhia cov ncov (001) thiab (002) ntawm ~ 23.5 ° thiab ~ 47.5 °, raws li, uas yog tus yam ntxwv ntawm nonstoichiometric WO2.63 (W32O84) (PDF 077–0810, a = 21.4 Å, b = 17.8 Å, c = 3.8 Å, α = β = γ = 90 °), uas sib raug rau lawv cov xim xiav ntshiab (Daim duab 1b) 48.49. Lwm cov ncov ntawm kwv yees li 20.5 °, 27.1 °, 28.1 °, 30.8 °, 35.7 °, 36.7 ° thiab 52.7 ° tau muab rau (140), (620), (350), (720), (740), (560 °). ) ) thiab (970) diffraction dav hlau orthogonal rau WO2.63, raws li. Songara et al. 43 siv tib txoj kev tsim khoom siv los ntawm kom tau txais cov khoom dawb, uas tau muab rau qhov muaj WO3 (H2O) 0.333. Txawm li cas los xij, hauv txoj haujlwm no, vim muaj ntau yam xwm txheej sib txawv, cov khoom xiav-grey tau txais, qhia tias WO3 (H2O) 0.333 (PDF 087-1203, a = 7.3 Å, b = 12.5 Å, c = 7.7 Å, α = β = γ = 90 °) thiab daim ntawv txo qis ntawm tungsten oxide. Kev tshuaj xyuas semiquantitative siv X'Pert HighScore software qhia 26% WO3 (H2O) 0.333: 74% W32O84. Vim tias W32O84 muaj W6+ thiab W4+ (1.67:1 W6+:W4+), cov ntsiab lus kwv yees ntawm W6+ thiab W4+ yog li 72% W6+ thiab 28% W4+, raws li. Cov duab SEM, 1-thib ob XPS spectra ntawm qib nucleus, TEM cov duab, FTIR spectra, thiab Raman spectra ntawm C76 cov khoom me me tau nthuav tawm hauv peb tsab xov xwm dhau los. Raws li Kawada et al.,50,51 X-ray diffraction ntawm C76 tom qab tshem tawm toluene qhia tau hais tias muaj cov qauv monoclinic ntawm FCC.
Cov duab SEM hauv daim duab 2a thiab b qhia tias HWO thiab HWO-50%C76 tau raug tso rau ntawm thiab ntawm cov carbon fibers ntawm UCC electrode. Cov duab qhia txog EDX ntawm tungsten, carbon, thiab oxygen ntawm cov duab SEM hauv daim duab 2c tau pom hauv daim duab 2d-f qhia tias tungsten thiab carbon tau sib xyaw sib npaug (qhia txog kev faib tawm zoo sib xws) hla tag nrho qhov chaw electrode thiab cov khoom sib xyaw tsis tau tso rau hauv qhov sib npaug vim yog qhov xwm txheej ntawm txoj kev tso tawm.
Cov duab SEM ntawm cov khoom me me HWO uas tau tso rau hauv (a) thiab cov khoom me me HWO-C76 (b). Daim duab qhia EDX ntawm HWO-C76 uas tau thauj khoom rau ntawm UCC siv thaj chaw hauv daim duab (c) qhia txog kev faib tawm ntawm tungsten (d), carbon (e), thiab oxygen (f) hauv cov qauv.
HR-TEM tau siv rau kev thaij duab loj thiab cov ntaub ntawv crystallographic (Daim Duab 3). HWO qhia txog cov qauv nanocube raws li pom hauv Daim Duab 3a thiab pom tseeb dua hauv Daim Duab 3b. Los ntawm kev ua kom lub nanocube loj dua rau kev diffraction ntawm cov cheeb tsam xaiv, ib tus tuaj yeem pom cov qauv grating thiab cov dav hlau diffraction uas ua tiav txoj cai Bragg, raws li pom hauv Daim Duab 3c, uas lees paub qhov crystallinity ntawm cov khoom. Hauv daim duab ntxig rau Daim Duab 3c qhia qhov deb d 3.3 Å sib raug rau (022) thiab (620) diffraction dav hlau pom hauv WO3 (H2O) 0.333 thiab W32O84 theem, feem 43, 44, 49. Qhov no sib xws nrog XRD kev tshuaj xyuas piav qhia saum toj no (Daim Duab 1b) txij li qhov pom ntawm lub dav hlau grating deb d (Daim Duab 3c) sib raug rau qhov muaj zog tshaj plaws XRD ncov hauv HWO qauv. Cov nplhaib qauv kuj tau pom hauv daim duab 3d, qhov twg txhua lub nplhaib sib raug rau lub dav hlau sib cais. Cov dav hlau WO3 (H2O) 0.333 thiab W32O84 yog xim dawb thiab xiav, raws li, thiab lawv cov XRD peaks sib xws kuj tau qhia hauv daim duab 1b. Lub nplhaib thawj zaug qhia hauv daim duab nplhaib sib raug rau thawj lub ncov cim hauv tus qauv x-ray ntawm (022) lossis (620) diffraction dav hlau. Los ntawm (022) txog (402) rings, cov nqi d-spacing yog 3.30, 3.17, 2.38, 1.93, thiab 1.69 Å, sib xws nrog XRD tus nqi ntawm 3.30, 3.17, 2, 45, 1.93. thiab 1.66 Å, uas yog sib npaug rau 44, 45, raws li.
(a) daim duab HR-TEM ntawm HWO, (b) qhia ib daim duab loj dua. Cov duab ntawm cov dav hlau grating tau qhia nyob rau hauv (c), inset (c) qhia ib daim duab loj dua ntawm cov dav hlau thiab lub suab d ntawm 0.33 nm sib raug rau cov dav hlau (002) thiab (620). (d) HWO nplhaib qauv qhia cov dav hlau cuam tshuam nrog WO3 (H2O) 0.333 (dawb) thiab W32O84 (xiav).
Kev tshuaj xyuas XPS tau ua tiav los txiav txim siab qhov tshuaj lom neeg ntawm qhov chaw thiab lub xeev oxidation ntawm tungsten (Cov Duab S1 thiab 4). Qhov dav dav XPS scan spectrum ntawm cov synthesized HWO tau pom hauv Daim Duab S1, qhia txog qhov muaj tungsten. XPS narrow-scan spectra ntawm W 4f thiab O 1s core theem tau pom hauv Figs. 4a thiab b, feem. W 4f spectrum faib ua ob lub spin-orbit doublets sib raug rau lub zog khi ntawm W oxidation xeev. thiab W 4f7/2 ntawm 36.6 thiab 34.9 eV yog tus yam ntxwv ntawm W4+ xeev ntawm 40, feem.)0.333. Cov ntaub ntawv haum qhia tias cov feem pua ​​​​​​atomic ntawm W6+ thiab W4+ yog 85% thiab 15%, feem, uas ze rau cov nqi kwv yees los ntawm XRD cov ntaub ntawv xav txog qhov sib txawv ntawm ob txoj kev. Ob txoj kev muab cov ntaub ntawv ntau nrog qhov tseeb qis, tshwj xeeb tshaj yog XRD. Tsis tas li ntawd, ob txoj kev no tshuaj xyuas cov khoom sib txawv ntawm cov khoom siv vim XRD yog ib txoj kev loj thaum XPS yog ib txoj kev nto uas tsuas yog mus txog ob peb nanometers. Lub O 1s spectrum yog muab faib ua ob lub ncov ntawm 533 (22.2%) thiab 530.4 eV (77.8%). Thawj qhov sib raug rau OH, thiab qhov thib ob rau cov pa oxygen hauv lub lattice hauv WO. Qhov muaj OH functional pawg yog sib xws nrog cov khoom hydration ntawm HWO.
Ib qho kev tshuaj xyuas FTIR kuj tau ua rau ob qho qauv no los tshuaj xyuas qhov muaj cov pab pawg ua haujlwm thiab cov dej sib koom ua ke hauv cov qauv HWO hydrated. Cov txiaj ntsig qhia tau tias cov qauv HWO-50% C76 thiab FT-IR HWO cov txiaj ntsig zoo sib xws vim muaj HWO, tab sis qhov muaj zog ntawm cov ncov sib txawv vim muaj ntau yam qauv siv los npaj rau kev tshuaj xyuas (Daim duab 5a). ) HWO-50% C76 qhia tau tias txhua lub ncov, tshwj tsis yog lub ncov ntawm tungsten oxide, muaj feem cuam tshuam nrog fullerene 24. Cov ntsiab lus ntxaws hauv daim duab 5a qhia tau tias ob qho qauv qhia txog cov kab dav dav heev ntawm ~ 710 / cm uas yog vim OWO ncab oscillations hauv HWO lattice qauv, nrog lub xub pwg nyom muaj zog ntawm ~ 840 / cm uas yog vim WO. Rau kev ncab vibrations, ib txoj kab ntse ntawm txog 1610 / cm yog vim khoov vibrations ntawm OH, thaum lub dav absorption band ntawm txog 3400 / cm yog vim ncab vibrations ntawm OH hauv hydroxyl pawg 43. Cov txiaj ntsig no sib xws nrog XPS spectra hauv Figs. 4b, qhov twg WO functional pawg tuaj yeem muab cov chaw nquag rau VO2+/VO2+ reaction.
Kev tshuaj xyuas FTIR ntawm HWO thiab HWO-50% C76 (a), qhia txog cov pab pawg ua haujlwm thiab kev ntsuas lub kaum sab xis (b, c).
Pawg OH kuj tseem tuaj yeem ua rau VO2+/VO2+ ua haujlwm, thaum ua rau hydrophilicity ntawm lub electrode nce ntxiv, yog li txhawb nqa qhov nrawm ntawm kev sib kis thiab kev hloov pauv hluav taws xob. Raws li qhia, HWO-50% C76 qauv qhia txog qhov siab tshaj plaws rau C76. Cov siab tshaj plaws ntawm ~ 2905, 2375, 1705, 1607, thiab 1445 cm3 tuaj yeem muab rau CH, O = C = O, C = O, C = C, thiab CO ncab kev co, raws li. Nws paub zoo tias cov pa oxygen ua haujlwm pawg C = O thiab CO tuaj yeem ua haujlwm ua cov chaw ua haujlwm rau cov tshuaj redox ntawm vanadium. Txhawm rau sim thiab sib piv qhov wettability ntawm ob lub electrodes, kev ntsuas lub kaum sab xis tau coj raws li qhia hauv daim duab 5b, c. Lub HWO electrode tam sim ntawd nqus cov dej ntws, qhia txog superhydrophilicity vim muaj OH ua haujlwm pawg. HWO-50% C76 yog hydrophobic ntau dua, nrog lub kaum sab xis ntawm txog 135 ° tom qab 10 vib nas this. Txawm li cas los xij, hauv kev ntsuas electrochemical, HWO-50%C76 electrode tau ntub tag hauv tsawg dua ib feeb. Kev ntsuas qhov ntub dej yog sib xws nrog XPS thiab FTIR cov txiaj ntsig, qhia tias ntau OH pawg ntawm HWO nto ua rau nws hydrophilic dua.
Cov tshuaj tiv thaiv VO2+/VO2+ ntawm HWO thiab HWO-C76 nanocomposites tau raug sim thiab nws xav tias HWO yuav tiv thaiv kev hloov pauv chlorine hauv VO2+/VO2+ tshuaj tiv thaiv hauv cov kua qaub sib xyaw, thiab C76 yuav ua rau cov tshuaj tiv thaiv VO2+/VO2+ redox xav tau ntxiv. %, 30%, thiab 50% C76 hauv HWO cov tshuaj ncua thiab CCC tso rau ntawm cov electrodes nrog tag nrho cov khoom thauj ntawm kwv yees li 2 mg / cm2.
Raws li pom hauv daim duab 6, qhov kinetics ntawm VO2+/VO2+ tshuaj tiv thaiv ntawm qhov electrode nto tau kuaj xyuas los ntawm CV hauv cov electrolyte acidic sib xyaw. Cov dej ntws tau qhia ua I/Ipa rau kev sib piv yooj yim ntawm ΔEp thiab Ipa/Ipc rau cov catalysts sib txawv ncaj qha rau ntawm daim duab. Cov ntaub ntawv tam sim no tau qhia hauv Daim Duab 2S. Ntawm daim duab 6a qhia tau hais tias HWO me ntsis ua rau tus nqi hloov pauv electron ntawm VO2+/VO2+ redox tshuaj tiv thaiv ntawm qhov electrode nto thiab tiv thaiv cov tshuaj tiv thaiv ntawm parasitic chlorine evolution. Txawm li cas los xij, C76 ua rau tus nqi hloov pauv electron ntau ntxiv thiab ua rau cov tshuaj tiv thaiv chlorine evolution. Yog li ntawd, cov khoom sib xyaw ua ke ntawm HWO thiab C76 raug xav tias yuav muaj kev ua haujlwm zoo tshaj plaws thiab muaj peev xwm zoo tshaj plaws los tiv thaiv cov tshuaj tiv thaiv chlorine evolution. Nws tau pom tias tom qab nce cov ntsiab lus ntawm C76, cov haujlwm electrochemical ntawm cov electrodes tau zoo dua, raws li pom los ntawm kev txo qis hauv ΔEp thiab kev nce hauv Ipa/Ipc piv (Rooj S3). Qhov no kuj tau lees paub los ntawm RCT tus nqi rho tawm los ntawm Nyquist daim duab hauv daim duab 6d (Rooj S3), uas tau pom tias txo qis nrog kev nce ntxiv ntawm C76 cov ntsiab lus. Cov txiaj ntsig no kuj sib xws nrog Li txoj kev tshawb fawb, uas qhov ntxiv ntawm mesoporous carbon rau mesoporous WO3 tau qhia txog kev hloov pauv kinetics ntawm VO2 + / VO2 + 35. Qhov no qhia tau hais tias qhov kev cuam tshuam ncaj qha yuav nyob ntawm qhov electrode conductivity (C = C bond) 18, 24, 35, 36, 37. Qhov no kuj tseem yuav yog vim muaj kev hloov pauv hauv kev sib koom tes geometry ntawm [VO (H2O) 5] 2 + thiab [VO2 (H2O) 4] +, C76 txo cov tshuaj tiv thaiv overvoltage los ntawm kev txo cov ntaub so ntswg lub zog. Txawm li cas los xij, qhov no yuav tsis ua tau nrog HWO electrodes.
(a) Cyclic voltammetric tus cwj pwm (ν = 5 mV/s) ntawm VO2+/VO2+ cov tshuaj tiv thaiv ntawm UCC thiab HWO-C76 composites nrog cov piv sib txawv HWO:C76 hauv 0.1 M VOSO4/1 M H2SO4 + 1 M HCl electrolyte. (b) Randles-Sevchik thiab (c) Nicholson VO2+/VO2+ txoj kev los ntsuas qhov ua tau zoo ntawm kev sib kis thiab tau txais cov nqi k0(d).
Tsis yog HWO-50% C76 tsuas yog ua kom pom zoo li qub electrocatalytic activity li C76 rau VO2+/VO2+ reaction xwb, tab sis, qhov nthuav dua, nws ntxiv rau suppressed chlorine evolution piv rau C76, raws li pom hauv daim duab 6a, thiab kuj qhia txog Lub voj voog me me hauv daim duab 6d (RCT qis dua). C76 tau pom Ipa/Ipc ntau dua li HWO-50% C76 (Rooj S3), tsis yog vim muaj kev hloov pauv zoo dua, tab sis vim yog qhov sib tshooj siab tshaj plaws ntawm chlorine txo cov tshuaj tiv thaiv nrog SHE ntawm 1.2 V. Kev ua tau zoo tshaj plaws ntawm HWO- 50% C76 yog vim muaj kev sib koom ua ke ntawm cov khoom siv hluav taws xob tsis zoo C76 thiab qhov dej siab thiab W-OH catalytic functionality ntawm HWO. Kev tso tawm chlorine tsawg dua yuav txhim kho qhov kev them nqi ntawm tag nrho lub cell, thaum kev txhim kho kinetics yuav txhim kho qhov ua tau zoo ntawm tag nrho lub cell voltage.
Raws li kab zauv S1, rau qhov kev cuam tshuam quasi-reversible (qeeb qeeb hloov hluav taws xob) tswj los ntawm diffusion, qhov siab tshaj plaws tam sim no (IP) nyob ntawm tus lej ntawm cov electrons (n), thaj tsam electrode (A), diffusion coefficient (D), tus lej ntawm cov electrons hloov coefficient (α) thiab scanning speed (ν). Txhawm rau kawm txog kev coj tus cwj pwm diffusion-controlled ntawm cov ntaub ntawv sim, kev sib raug zoo ntawm IP thiab ν1/2 tau plotted thiab nthuav tawm hauv daim duab 6b. Txij li thaum txhua yam ntaub ntawv qhia txog kev sib raug zoo linear, qhov kev cuam tshuam yog tswj los ntawm diffusion. Txij li thaum VO2+/VO2+ kev cuam tshuam yog quasi-reversible, qhov nqes hav ntawm kab nyob ntawm qhov diffusion coefficient thiab tus nqi ntawm α (kab zauv S1). Txij li thaum diffusion coefficient yog tas li (≈ 4 × 10–6 cm2/s)52, qhov sib txawv ntawm qhov nqes hav ntawm kab ncaj qha qhia txog cov nqi sib txawv ntawm α, thiab yog li ntawd qhov hloov hluav taws xob ntawm qhov electrode nto, uas tau qhia rau C76 thiab HWO -50% C76 Qhov nqes hav ntxhab tshaj plaws (qhov hloov hluav taws xob siab tshaj plaws).
Cov Warburg slopes (W) xam rau cov zaus qis uas tau qhia hauv Rooj S3 (Daim duab 6d) muaj cov nqi ze rau 1 rau txhua yam khoom siv, qhia txog kev sib kis zoo meej ntawm cov hom redox thiab lees paub qhov kev coj cwj pwm ntawm IP piv rau ν1/2. CV raug ntsuas. Rau HWO-50% C76, Warburg slope deviates ntawm 1 mus rau 1.32, qhia tsis yog tsuas yog semi-infinite diffusion ntawm cov reagent (VO2+), tab sis kuj yog qhov ua tau ntawm cov cwj pwm nyias-txheej rau kev coj cwj pwm diffusion vim yog electrode porosity.
Txhawm rau txheeb xyuas ntxiv txog qhov rov qab hloov pauv (electron transfer rate) ntawm VO2+/VO2+ redox reaction, Nicholson quasi-reversible reaction method kuj tau siv los txiav txim siab tus nqi tas li k041.42. Qhov no ua tiav siv S2 equation los tsim cov dimensionless kinetic parameter Ψ, uas yog ib qho function ntawm ΔEp, ua ib qho function ntawm ν-1/2. Rooj S4 qhia cov nqi Ψ tau txais rau txhua cov khoom siv electrode. Cov txiaj ntsig (Daim duab 6c) tau plotted kom tau k0 × 104 cm/s los ntawm qhov nqes hav ntawm txhua daim duab siv Equation S3 (sau ib sab ntawm txhua kab thiab nthuav tawm hauv Rooj S4). HWO-50% C76 tau pom tias muaj qhov nqes hav siab tshaj plaws (Daim duab 6c), yog li tus nqi siab tshaj plaws ntawm k0 yog 2.47 × 10–4 cm/s. Qhov no txhais tau hais tias lub electrode no ua tiav qhov kinetics ceev tshaj plaws, uas yog sib xws nrog CV thiab EIS cov txiaj ntsig hauv daim duab 6a thiab d thiab hauv Rooj S3. Tsis tas li ntawd, tus nqi ntawm k0 kuj tau txais los ntawm Nyquist plot (Daim duab 6d) ntawm Equation S4 siv tus nqi RCT (Rooj S3). Cov txiaj ntsig k0 no los ntawm EIS tau muab sau ua ke hauv Rooj S4 thiab kuj qhia tias HWO-50% C76 qhia txog tus nqi hloov pauv hluav taws xob siab tshaj plaws vim yog qhov cuam tshuam synergistic. Txawm hais tias cov nqi k0 txawv vim yog keeb kwm sib txawv ntawm txhua txoj kev, lawv tseem qhia tib qho kev txiav txim ntawm qhov loj me thiab qhia txog kev sib xws.
Yuav kom nkag siab tag nrho cov kinetics zoo heev uas tau txais, nws yog ib qho tseem ceeb uas yuav tsum sib piv cov khoom siv electrode zoo tshaj plaws nrog cov electrodes UCC thiab TCC uas tsis tau coated. Rau qhov VO2 + / VO2 + tshuaj tiv thaiv, HWO-C76 tsis yog tsuas yog qhia qhov qis tshaj plaws ΔEp thiab zoo dua reversibility, tab sis kuj tseem ceeb suppressed qhov parasitic chlorine evolution reaction piv rau TCC, raws li ntsuas los ntawm tam sim no ntawm 1.45 V piv rau SHE (Daim duab 7a). Hais txog kev ruaj khov, peb xav tias HWO-50% C76 ruaj khov vim tias cov catalyst tau sib xyaw nrog PVDF binder thiab tom qab ntawd siv rau cov ntaub carbon electrodes. HWO-50% C76 tau qhia txog qhov hloov pauv siab tshaj plaws ntawm 44 mV (degradation rate 0.29 mV / voj voog) tom qab 150 voj voog piv rau 50 mV rau UCC (Daim duab 7b). Qhov no yuav tsis yog qhov sib txawv loj, tab sis kinetics ntawm UCC electrodes qeeb heev thiab degrades nrog kev caij tsheb kauj vab, tshwj xeeb tshaj yog rau cov tshuaj tiv thaiv rov qab. Txawm hais tias qhov kev hloov pauv ntawm TCC zoo dua li ntawm UCC, TCC tau pom tias muaj qhov hloov pauv loj ntawm 73 mV tom qab 150 lub voj voog, uas tej zaum yuav yog vim muaj ntau cov chlorine tsim rau ntawm nws qhov chaw. yog li ntawd cov catalyst lo rau ntawm qhov chaw electrode zoo. Raws li tuaj yeem pom los ntawm txhua lub electrodes sim, txawm tias cov electrodes tsis muaj cov catalysts txhawb nqa tau qhia txog ntau qib ntawm kev tsis ruaj khov ntawm kev sib tw, qhia tias qhov kev hloov pauv ntawm qhov sib cais thaum lub sijhawm sib tw yog vim kev ua haujlwm ntawm cov khoom siv los ntawm kev hloov pauv tshuaj es tsis yog kev sib cais catalyst. Tsis tas li ntawd, yog tias muaj ntau cov khoom catalyst raug cais tawm ntawm qhov chaw electrode, qhov no yuav ua rau muaj kev nce ntxiv ntawm qhov sib cais ncov (tsis yog 44 mV xwb), txij li thaum lub substrate (UCC) tsis tshua muaj zog rau VO2 + / VO2 + redox reaction.
Kev sib piv ntawm CV ntawm cov khoom siv electrode zoo tshaj plaws piv rau UCC (a) thiab kev ruaj khov ntawm VO2 + / VO2 + redox reaction (b). ν = 5 mV / s rau txhua CVs hauv 0.1 M VOSO4 / 1 M H2SO4 + 1 M HCl electrolyte.
Yuav kom ua rau VRFB thev naus laus zis zoo dua, kev nthuav dav thiab kev nkag siab txog kinetics ntawm vanadium redox reactions yog qhov tseem ceeb kom ua tiav kev siv hluav taws xob zoo. Composites HWO-C76 tau npaj thiab lawv cov nyhuv electrocatalytic ntawm VO2 + / VO2 + reaction tau kawm. HWO tau qhia me ntsis kinetic txhim kho hauv cov electrolytes acidic sib xyaw tab sis tseem ceeb suppressed chlorine evolution. Ntau yam piv ntawm HWO: C76 tau siv los txhim kho ntxiv kinetics ntawm HWO-raws li electrodes. Kev nce C76 rau HWO txhim kho cov electron hloov kinetics ntawm VO2 + / VO2 + reaction ntawm lub electrode hloov kho, uas HWO-50% C76 yog cov khoom zoo tshaj plaws vim nws txo cov nqi hloov pauv tsis kam thiab ntxiv suppresses chlorine piv rau C76 thiab TCC deposit. . Qhov no yog vim muaj cov nyhuv synergistic ntawm C = C sp2 hybridization, OH thiab W-OH functional pawg. Tus nqi degradation tom qab rov ua dua ntawm HWO-50% C76 tau pom tias yog 0.29 mV / voj voog, thaum tus nqi degradation ntawm UCC thiab TCC yog 0.33 mV / voj voog thiab 0.49 mV / voj voog, ua rau nws ruaj khov heev. hauv cov electrolytes sib xyaw ua ke. Cov txiaj ntsig tau nthuav tawm tau txheeb xyuas cov khoom siv electrode ua tau zoo rau VO2 + / VO2 + tshuaj tiv thaiv nrog kinetics ceev thiab ruaj khov siab. Qhov no yuav ua rau lub zog tso zis ntau ntxiv, yog li ua rau lub zog ua haujlwm ntawm VRFB nce ntxiv, yog li txo tus nqi ntawm nws cov lag luam yav tom ntej.
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