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Qiimaha sare ee baytariyada redox-ka ee dhammaan vanadium-ka (VRBBs) ayaa xaddidaya isticmaalkooda ballaaran. Hagaajinta kinetics-ka falgallada electrochemical ayaa loo baahan yahay si loo kordhiyo awoodda gaarka ah iyo hufnaanta tamarta ee VRFB, taasoo yareynaysa kharashka kWh ee VRFB. Shaqadan, nanoparticles-ka tungsten oxide (HWO) ee hydrothermally synthesized hydrothermally synthesized, C76 iyo C76/HWO, ayaa lagu shubay elektroodhyada maro kaarboonka waxaana lagu tijaabiyay sidii electrocatalysts for reaction redox VO2+/VO2+. Microscopy-ga elektaroonigga ah ee iskaanka qiiqa goobta (FESEM), spectroscopy-ga X-ray-ga ee kala firdhisan (EDX), microscopy-ga elektaroonigga gudbinta ee xallinta sare leh (HR-TEM), kala-soocidda X-ray (XRD), spectroscopy-ga sawir-qaadista X-ray (XPS), infrared Fourier transform Spectroscopy (FTIR) iyo cabbiraadaha xagasha xiriirka. Waxaa la ogaaday in ku darista C76 fullerenes ee HWO ay hagaajin karto kinetics-ka elektiroonigga ah iyadoo kordhinaysa socodka korantada iyo bixinta kooxo shaqeynaya oo oksaydhaysan oo dusha sare ah, taasoo kor u qaadaysa falcelinta redox-ka VO2+/VO2+. Isku-darka HWO/C76 (50 wt% C76) wuxuu noqday doorashada ugu fiican ee falcelinta VO2+/VO2+ oo leh ΔEp oo ah 176 mV, halka maro kaarboon ah oo aan la daaweyn (UCC) ay ahayd 365 mV. Intaa waxaa dheer, isku-darka HWO/C76 wuxuu muujiyay saameyn xakameyn ah oo muhiim ah oo ku saabsan falcelinta isbeddelka koloriin-ka ee dulinka ah sababtoo ah kooxda shaqaynaysa ee W-OH.
Dhaqdhaqaaqa xooggan ee aadanaha iyo kacaanka warshadaha ee degdegga ah ayaa horseeday baahida korontada oo aad u sarreysa, taasoo sii kordheysa qiyaastii 3% sannadkiiba1. Tobannaan sano, isticmaalka baahsan ee shidaalka fosil ahaan il tamar ahaan ayaa horseeday qiiqa gaaska aqalka dhirta lagu koriyo oo gacan ka geysta kulaylka caalamiga ah, wasakhowga biyaha iyo hawada, taasoo halis gelinaysa dhammaan nidaamyada deegaanka. Natiijo ahaan, gelitaanka dabaysha nadiifka ah iyo tamarta qorraxda ayaa la filayaa inay gaarto 75% wadarta korontada marka la gaaro 20501. Si kastaba ha ahaatee, marka saamiga korontada ee ka timaadda ilaha la cusboonaysiin karo uu ka bato 20% wadarta guud ee korontada, shabakadu waxay noqotaa mid aan degganayn.
Dhammaan nidaamyada kaydinta tamarta sida battery-ga isku-dhafka ah ee vanadium redox flow2, baytariga socodka redox-ka ee dhammaan-vanadium (VRFB) ayaa si dhakhso leh u horumaray sababtoo ah faa'iidooyinkiisa badan waxaana loo arkaa xalka ugu fiican kaydinta tamarta muddada dheer (qiyaastii 30 sano).) Xulashooyinka oo ay weheliso tamarta la cusboonaysiin karo4. Tani waxay sabab u tahay kala-soocidda cufnaanta awoodda iyo tamarta, jawaab celinta degdegga ah, cimriga adeegga dheer, iyo kharash sannadeed hooseeya oo ah $65/kWh marka la barbar dhigo $93-140/kWh ee baytariyada Li-ion iyo lead-acid iyo 279-420 doolarka Mareykanka halkii kWh. baytariga siday u kala horreeyaan 4.
Si kastaba ha ahaatee, ganacsigooda baaxadda weyn ayaa wali ku xiran kharashkooda raasamaalka nidaamka oo aad u sarreeya, inta badan sababtoo ah xirmooyinka unugyada4,5. Sidaa darteed, hagaajinta waxqabadka kaydka iyadoo la kordhinayo kinetics-ka labada falgallo ee nus-element waxay yareyn kartaa cabbirka kaydka sidaas darteedna waxay yareyn kartaa kharashka. Sidaa darteed, wareejinta elektarooniga si degdeg ah ugu socota dusha sare ee elektroodka ayaa lagama maarmaan ah, taas oo ku xidhan naqshadaynta, halabuurka iyo qaab-dhismeedka elektroodka waxayna u baahan tahay hagaajin taxaddar leh6. Iyadoo ay jirto xasilloonida kiimikada iyo elektroodka wanaagsan iyo gudbinta korontada ee wanaagsan ee elektroodka kaarboonka, kinetics-kooda aan la daaweyn waa gaabis sababtoo ah maqnaanshaha kooxaha shaqeynaya ee oksijiinta iyo hydrophilicity7,8. Sidaa darteed, electrocatalysts kala duwan ayaa lagu daraa elektroodhada ku salaysan kaarboonka, gaar ahaan nanostructures-ka kaarboonka iyo oksaydhyada birta, si loo hagaajiyo kinetics-ka labada elektroodka, taasoo kordhinaysa kinetics-ka elektroodka VRFB.
Marka laga soo tago shaqadeennii hore ee C76, waxaan marka hore soo sheegnay dhaqdhaqaaqa korantada ee aadka u fiican ee fullerene-kan ee VO2+/VO2+, wareejinta dallacaadda, marka la barbar dhigo maro kaarboon ah oo lagu daweeyay kulaylka iyo kuwa aan la daweyn. Iska caabbinta waxaa hoos u dhacday 99.5% iyo 97%. Waxqabadka katalytic-ga ee walxaha kaarboonka ee falcelinta VO2+/VO2+ marka la barbar dhigo C76 waxaa lagu muujiyay Shaxda S1. Dhanka kale, oksaydhyo bir ah oo badan sida CeO225, ZrO226, MoO327, NiO28, SnO229, Cr2O330 iyo WO331, 32, 33, 34, 35, 36, 37 ayaa la isticmaalay sababtoo ah qoyaankooda oo kordhay iyo shaqada oksijiinta oo badan. , 38. Dhaqdhaqaaqa katalytic-ga ee oksaydhyadan birta ah ee falcelinta VO2+/VO2+ waxaa lagu soo bandhigay Shaxda S2. WO3 waxaa loo isticmaalay tiro badan oo shaqooyin ah sababtoo ah kharash yar, xasillooni sare oo ku jirta warbaahinta aashitada leh, iyo dhaqdhaqaaqa kicinta sare31,32,33,34,35,36,37,38. Si kastaba ha ahaatee, horumarinta kinetics-ka cathodic ee ay keento WO3 waa mid aan muhiim ahayn. Si loo hagaajiyo socodka WO3, saameynta isticmaalka tungsten oxide (W18O49) oo yaraaday dhaqdhaqaaqa cathodic ayaa la tijaabiyay38. Tungsten oxide (HWO) oo la qaboojiyey waligiis laguma tijaabin codsiyada VRFB, inkastoo ay muujinayso firfircooni kordhaysa codsiyada supercapacitor sababtoo ah faafinta cation ee degdega ah marka la barbar dhigo WOx39,40 oo aan biyo lahayn. Baytariga socodka vanadium redox ee jiilka saddexaad wuxuu isticmaalaa elektrolyt isku dhafan oo aashitada ah oo ka kooban HCl iyo H2SO4 si loo hagaajiyo waxqabadka batteriga loona hagaajiyo milmida iyo xasilloonida ions vanadium ee elektrolaytka. Si kastaba ha ahaatee, falcelinta isbeddelka koloriinka ee dulinka ah ayaa noqotay mid ka mid ah faa'iidooyinka jiilka saddexaad, sidaa darteed raadinta siyaabo lagu joojiyo falcelinta qiimaynta koloriinka ayaa noqotay diiradda kooxo cilmi-baaris oo dhowr ah.
Halkan, tijaabooyinka falcelinta VO2+/VO2+ waxaa lagu sameeyay isku-darka HWO/C76 ee lagu shubay elektroodhada maro kaarboon si loo helo dheelitir u dhexeeya socodka korantada ee isku-darka iyo kinetics-ka redox ee dusha sare ee elektroodka iyadoo la xakameynayo isbeddelka koloriin-ka dulinka ah. jawaab celinta (CER). Nanoparticles-ka tungsten oxide (HWO) ee la qalajiyey waxaa lagu sameeyay hab hydrothermal fudud. Tijaabooyinka waxaa lagu sameeyay elektroolayt isku dhafan oo aashito ah (H2SO4/HCl) si loogu daydo jiilka saddexaad ee VRFB (G3) si loo helo wax ku oolnimo iyo in la baaro saameynta HWO ee falcelinta isbeddelka koloriin-ka dulinka ah.
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) iyo maro kaarboon hydrophilic ah ELAT (Shidaalka Unugyada Shidaalka) ayaa loo isticmaalay daraasaddan.
Oxide tungsten ah oo la qalajiyey (HWO) waxaa lagu diyaariyey falgalka hydrothermal 43 kaas oo 2 g oo milix ah oo Na2WO4 ah lagu milmay 12 ml oo H2O ah si loo siiyo xal aan midab lahayn, ka dibna 12 ml oo 2 M HCl ah ayaa lagu daray hoos u dhac si loo siiyo suuxdin huruud khafiif ah. Slurry-ka waxaa lagu riday autoclave bir ah oo aan miridh lahayn oo Teflon lagu dahaadhay waxaana lagu hayaa foorno heerkulkeedu yahay 180°C. muddo 3 saacadood ah si loogu falceliyo hydrothermal. Hadhaaga waxaa lagu ururiyay shaandhayn, saddex jeer ayaa lagu dhaqay ethanol iyo biyo, waxaana lagu qalajiyey foorno heerkulkeedu yahay 70°C muddo ~3 saacadood ah, ka dibna waxaa lagu shubay si loo helo budo HWO oo buluug-cawlan ah.
Elektroodhada maro kaarboonka ee la helay (aan la daweyn) (CCT) waxaa loo isticmaalay sidii loogu talagalay ama kuleylka lagu daweeyay foorno tuubo ah oo heerkulkeedu yahay 450°C hawada iyadoo heerkulku yahay 15 ºC/daqiiqo muddo 10 saacadood ah si loo helo CCs la daweeyay (TCC). sida lagu sharaxay maqaalkii hore24. UCC iyo TCC waxaa loo jaray elektroodhada qiyaastii 1.5 cm ballac iyo 7 cm dheer. Joojinta C76, HWO, HWO-10% C76, HWO-30% C76 iyo HWO-50% C76 waxaa la diyaariyey iyadoo lagu daray 20 mg .% (~2.22 mg) oo ah xidhmada PVDF ilaa ~1 ml DMF waxaana la isku daray 1 saac si loo hagaajiyo isku-dhafka. 2 mg oo ah isku-darka C76, HWO iyo HWO-C76 ayaa si isdaba joog ah loogu dabaqay aagga elektroodka firfircoon ee UCC oo qiyaastii ah 1.5 cm2. Dhammaan kiciyeyaasha waxaa lagu shubay elektroodhada UCC, TCC-na waxaa loo isticmaalay ujeeddooyin isbarbardhig oo keliya, maadaama shaqadeennii hore ay muujisay in daaweynta kulaylka aan loo baahnayn24. Dejinta aragtida waxaa lagu gaaray iyadoo la cadayo 100 µl oo ka mid ah joojinta (culayska 2 mg) si loo helo saameyn siman. Kadib dhammaan elektroodhada waxaa lagu qalajiyey foorno heerkul ah 60° C. habeenkii. Elektroodhada waxaa lagu cabbiraa hore iyo gadaal si loo hubiyo rarista saxda ah ee kaydka. Si loo helo aag joomatari ah oo gaar ah (~1.5 cm2) loogana hortago kor u kaca elektroollada vanadium ee elektroodka sababtoo ah saameynta xididka, lakab khafiif ah oo paraffin ah ayaa lagu mariyey walxaha firfircoon.
Mikroskoobka elektarooniga ee iskaanka qiiqa goobta (FESEM, Zeiss SEM Ultra 60, 5 kV) ayaa loo isticmaalay in lagu eego qaab-dhismeedka dusha sare ee HWO. Mikroskoob X-ray ah oo kala firdhiya tamarta oo ku qalabaysan Feii8SEM (EDX, Zeiss Inc.) ayaa loo isticmaalay in lagu sawiro walxaha HWO-50%C76 ee ku yaal elektroodhada UCC. Mikroskoob elektaroonig ah oo gudbin ah oo xallin sare leh (HR-TEM, JOEL JEM-2100) oo ku shaqeeya danab xawaare sare leh oo ah 200 kV ayaa loo isticmaalay in lagu sawiro walxaha HWO ee xallinta sare leh iyo giraangiraha kala-soocidda. Barnaamijka Qalabka Crystallography (CrysTBox) wuxuu adeegsadaa shaqada ringGUI si uu u falanqeeyo qaabka kala-soocidda giraanta HWO oo uu natiijooyinka u barbar dhigo qaabka XRD. Qaab-dhismeedka iyo garaafka UCC iyo TCC waxaa lagu falanqeeyay kala-soocidda raajada (XRD) iyadoo lagu sameeyay heerka sawir-qaadista 2.4°/daqiiqo laga bilaabo 5° ilaa 70° iyadoo la adeegsanayo Cu Kα (λ = 1.54060 Å) iyadoo la adeegsanayo cabbiraha raajada ee Panalytical X-ray diffractometer (Model 3600). XRD waxay muujisay qaab-dhismeedka kiristaalka iyo marxaladda HWO. Barnaamijka PANAlytical X'Pert HighScore waxaa loo isticmaalay in lagu waafajiyo meelaha ugu sarreeya HWO iyo khariidadaha tungsten oxide ee laga heli karo xogta45. Natiijooyinka HWO waxaa la barbar dhigay natiijooyinka TEM. Halabuurka kiimikada iyo xaaladda muunadaha HWO waxaa lagu go'aamiyay sawir-qaadista sawir-qaadista sawir-qaadista X-ray (XPS, ESCALAB 250Xi, ThermoScientific). Barnaamijka CASA-XPS (v 2.3.15) waxaa loo isticmaalay kala-soocidda ugu sarreysa iyo falanqaynta xogta. Si loo go'aamiyo kooxaha shaqada dusha sare ee HWO iyo HWO-50%C76, cabbiraadaha waxaa lagu sameeyay iyadoo la adeegsanayo Fourier transform infrared spectroscopy (FTIR, Perkin Elmer spectrometer, iyadoo la adeegsanayo KBr FTIR). Natiijooyinka waxaa la barbar dhigay natiijooyinka XPS. Cabbiraadaha xagasha xiriirka (KRUSS DSA25) ayaa sidoo kale loo isticmaalay in lagu qeexo qoyaanka elektroodhada.
Dhammaan cabbiraadaha elektiroonigga ah, waxaa la isticmaalay goob shaqo oo Biologic SP 300 ah. Voltammetry-ga wareegga ah (CV) iyo electrochemical impedance spectroscopy (EIS) ayaa loo isticmaalay in lagu barto kinetics-ka elektiroonigga ee falgalka redox-ka VO2+/VO2+ iyo saameynta faafinta reagent-ka (VOSO4(VO2+)) ee heerka falgalka. Labada habba waxay isticmaaleen unug saddex-electrode ah oo leh fiirsashada elektiroonigga ah ee 0.1 M VOSO4 (V4+) ee 1 M H2SO4 + 1 M HCl (isku darka asiidhyada). Dhammaan xogta elektiroonigga ah ee la soo bandhigay waa la saxay IR. Elektrod calomel buuxa (SCE) iyo gariirad platinum (Pt) ah ayaa loo isticmaalay elektrod tixraac iyo ka-hortag, siday u kala horreeyaan. CV-ga, heerarka iskaanka (ν) ee 5, 20, iyo 50 mV/s ayaa lagu dabaqay daaqadda suurtagalka ah ee VO2+/VO2+ ee (0–1) V iyo SCE, ka dibna loo hagaajiyay SHE si ay u sawirto (VSCE = 0.242 V iyo HSE). Si loo barto haynta dhaqdhaqaaqa elektroodka, CV-yada wareega ee soo noqnoqda ayaa lagu sameeyay ν 5 mV/s ee UCC, TCC, UCC-C76, UCC-HWO, iyo UCC-HWO-50% C76. Cabbiraadaha EIS, heerka soo noqnoqda ee falcelinta redox ee VO2+/VO2+ wuxuu ahaa 0.01-105 Hz, iyo khalkhalka danabka ee danabka wareegga furan (OCV) wuxuu ahaa 10 mV. Tijaabo kasta waxaa lagu celceliyay 2-3 jeer si loo hubiyo isku dheelitirka natiijooyinka. Joogtada heerka kala duwan (k0) waxaa helay habka Nicholson46,47.
Oxide tungsten ah oo la qalajiyey (HVO) ayaa si guul leh loogu farsameeyey habka hydrothermal. Sawirka SEM ee jaantuska 1a wuxuu muujinayaa in HWO-ga la dhigay uu ka kooban yahay kooxo nanoparticles ah oo cabbirkoodu yahay 25-50 nm.
Qaabka kala-soocidda raajada ee HWO wuxuu muujinayaa meelaha ugu sarreeya (001) iyo (002) ~23.5° iyo ~47.5°, siday u kala horreeyaan, kuwaas oo astaan ​​u ah WO2.63 aan ahayn stoichiometric (W32O84) (PDF 077–0810, a = 21.4 Å, b = 17.8 Å, c = 3.8 Å, α = β = γ = 90°), taas oo u dhiganta midabkooda buluugga cad (Jaantuska 1b) 48.49. Meelaha kale ee ugu sarreeya qiyaastii 20.5°, 27.1°, 28.1°, 30.8°, 35.7°, 36.7° iyo 52.7° waxaa loo qoondeeyay (140), (620), (350), (720), (740), (560°). ) ) iyo (970) diyaaradaha kala-soocidda ee orthogonal ilaa WO2.63, siday u kala horreeyaan. Habka isku-dhafka ah waxaa isticmaalay Songara et al. 43 si loo helo badeecad cad, taas oo loo aaneeyay joogitaanka WO3(H2O)0.333. Si kastaba ha ahaatee, shaqadan, sababo la xiriira xaalado kala duwan, waxaa la helay badeecad buluug-cawlan ah, taasoo muujinaysa in WO3(H2O)0.333 (PDF 087-1203, a = 7.3 Å, b = 12.5 Å, c = 7 .7 Å, α = β = γ = 90°) iyo qaabka la dhimay ee tungsten oxide. Falanqaynta semiquantitative iyadoo la adeegsanayo barnaamijka X'Pert HighScore waxay muujisay 26% WO3(H2O)0.333:74% W32O84. Maadaama W32O84 uu ka kooban yahay W6+ iyo W4+ (1.67:1 W6+:W4+), qiyaasta ku jirta W6+ iyo W4+ waa qiyaastii 72% W6+ iyo 28% W4+, siday u kala horreeyaan. Sawirrada SEM, 1-ilbiriqsi oo XPS ah oo heerka xudunta ah, sawirrada TEM, FTIR spectra, iyo Raman spectra ee walxaha C76 ayaa lagu soo bandhigay maqaalkeennii hore. Sida laga soo xigtay Kawada et al., 50,51 Kala-soocidda X-ray ee C76 ka dib markii laga saaray toluene waxay muujisay qaab-dhismeedka monoclinic ee FCC.
Sawirada SEM ee jaantuska 2a iyo b waxay muujinayaan in HWO iyo HWO-50%C76 si guul leh loogu shubay oo u dhexeeya fiilooyinka kaarboon ee elektroodka UCC. Khariidadaha curiyaha EDX ee tungsten, kaarboon, iyo oksijiinta sawirada SEM ee jaantuska 2c waxaa lagu muujiyay jaantuska 2d-f taasoo muujinaysa in tungsten iyo kaarboonku si siman isugu qasan yihiin (oo muujinaya qaybin la mid ah) dusha sare ee elektroodka oo dhan oo isku-dhafka aan si isku mid ah loogu shubin sababtoo ah dabeecadda habka dhigista.
Sawirada SEM ee walxaha HWO ee la dhigay (a) iyo walxaha HWO-C76 (b). Khariidaynta EDX ee HWO-C76 ee lagu shubay UCC iyadoo la adeegsanayo aagga sawirka (c) waxay muujinaysaa qaybinta tungsten (d), kaarboon (e), iyo oksijiin (f) ee muunadda.
HR-TEM waxaa loo isticmaalay sawir-qaadista weynaynta sare iyo macluumaadka kiristaalka (Jaantuska 3). HWO waxay muujinaysaa qaab-dhismeedka nanocube sida ku cad Sawirka 3a iyo si ka sii cad Sawirka 3b. Marka la weyneeyo nanocube si loo kala saaro meelaha la doortay, qofku wuxuu arki karaa qaab-dhismeedka shabagga iyo diyaaradaha kala-soocidda ee buuxiya sharciga Bragg, sida ku cad Sawirka 3c, kaas oo xaqiijinaya kiristaalka walxaha. Qaybta hoose ee Sawirka 3c waxay muujinaysaa masaafada d 3.3 Å oo u dhiganta diyaaradaha kala-soocidda (022) iyo (620) ee laga helay marxaladaha WO3(H2O)0.333 iyo W32O84, siday u kala horreeyaan43,44,49. Tani waxay la jaanqaadaysaa falanqaynta XRD ee kor lagu sharaxay (Jaantuska 1b) maadaama masaafada diyaaradda shabagga ee la arkay d (Jaantuska 3c) ay u dhigantaa meesha ugu sarreysa XRD ee muunadda HWO. Faraantiyada muunadaha ayaa sidoo kale lagu muujiyay sawirka 3d, halkaas oo giraan kasta uu u dhigmo diyaarad gooni ah. Diyaaradaha WO3(H2O)0.333 iyo W32O84 waxay leeyihiin midab cad iyo buluug ah, siday u kala horreeyaan, meelaha ugu sarreeya ee XRD-koodana waxaa sidoo kale lagu muujiyay Jaantuska 1b. Faraantiga ugu horreeya ee lagu muujiyey jaantuska faraantiga wuxuu u dhigmaa meesha ugu sarreysa ee ugu horreysa ee calaamadaysan qaabka raajada ee diyaaradda kala-soocidda (022) ama (620). Laga bilaabo giraangiraha (022) ilaa (402), qiimayaasha kala-fogaanshaha d waa 3.30, 3.17, 2.38, 1.93, iyo 1.69 Å, oo la jaanqaadaya qiimayaasha XRD ee 3.30, 3.17, 2, 45, 1.93. iyo 1.66 Å, oo la mid ah 44, 45, siday u kala horreeyaan.
(a) Sawirka HR-TEM ee HWO, (b) wuxuu muujinayaa sawir la ballaariyay. Sawirada diyaaradaha shabagga waxaa lagu muujiyay (c), qaybta hoose (c) waxay muujinaysaa sawir la ballaariyay oo diyaaradaha ah iyo garaac d ah oo ah 0.33 nm oo u dhigma diyaaradaha (002) iyo (620). (d) Qaabka giraanta HWO oo muujinaya diyaaradaha la xiriira WO3(H2O)0.333 (caddaan) iyo W32O84 (buluug).
Falanqaynta XPS waxaa la sameeyay si loo go'aamiyo kiimikada dusha sare iyo xaaladda oksaydhka ee tungsten (Jaantusyada S1 iyo 4). Jaantuska baaritaanka XPS ee baaxadda ballaaran ee HWO ee la sameeyay waxaa lagu muujiyay Jaantuska S1, taasoo muujinaysa jiritaanka tungsten. Jaantuska baarista cidhiidhiga ah ee XPS ee heerarka asaasiga ah ee W 4f iyo O 1s waxaa lagu muujiyay Jaantusyada 4a iyo b, siday u kala horreeyaan. Jaantuska W 4f wuxuu u qaybsamaa laba labanlaab oo wareeg ah oo u dhigma tamarta isku xidhka ee xaaladda oksaydhka W. iyo W 4f7/2 ee 36.6 iyo 34.9 eV waa astaamo u ah xaaladda W4+ ee 40, siday u kala horreeyaan. )0.333. Xogta la rakibay waxay muujinaysaa in boqolleyda atomiga ee W6+ iyo W4+ ay yihiin 85% iyo 15%, siday u kala horreeyaan, kuwaas oo u dhow qiimayaasha laga qiyaasay xogta XRD iyadoo la tixgelinayo kala duwanaanshaha labada hab. Labada habba waxay bixiyaan macluumaad tiro leh oo leh saxnaan hoose, gaar ahaan XRD. Sidoo kale, labadan hab waxay falanqeeyaan qaybo kala duwan oo ka mid ah walxaha sababtoo ah XRD waa hab ballaaran halka XPS uu yahay hab dusha sare ah oo u dhow dhowr nanometer. Jaantuska O1s waxaa loo qaybiyaa laba meelood oo ugu sarreeya 533 (22.2%) iyo 530.4 eV (77.8%). Kan hore wuxuu u dhigmaa OH, kan labaadna wuxuu u dhigmaa isku xidhka oksijiinta ee shabagga WO. Joogitaanka kooxaha shaqeynaya ee OH waxay la jaan qaadayaan sifooyinka fuuq-celinta ee HWO.
Falanqaynta FTIR ayaa sidoo kale lagu sameeyay labadan muunadood si loo baaro joogitaanka kooxaha shaqeynaya iyo isku-dubaridka molecules-ka biyaha ee qaab-dhismeedka HWO ee qoyaanka leh. Natiijooyinka waxay muujinayaan in muunadda HWO-50% C76 iyo natiijooyinka FT-IR HWO ay u muuqdaan kuwo isku mid ah sababtoo ah joogitaanka HWO, laakiin xoojinta meelaha ugu sarreeya way kala duwan yihiin sababtoo ah xaddiga kala duwan ee muunadda loo isticmaalay diyaarinta falanqaynta (Jaantuska 5a).) HWO-50% C76 waxay muujinaysaa in dhammaan meelaha ugu sarreeya, marka laga reebo meesha ugu sarreysa ee tungsten oxide, ay la xiriiraan fullerene 24. Faahfaahinta jaantuska 5a waxay muujinaysaa in labada muunadoodba ay muujinayaan xarig ballaaran oo aad u xooggan oo ah ~710/cm oo loo aaneynayo gariirka fidinta OWO ee qaab-dhismeedka shabagga HWO, oo leh garab xooggan oo ah ~840/cm oo loo aaneynayo WO. Gariirka fidinta, xarig fiiqan oo ah qiyaastii 1610/cm waxaa loo aaneynayaa gariirka foorarsiga ee OH, halka xarig nuugis ballaaran oo ah qiyaastii 3400/cm waxaa loo aaneynayaa gariirka fidinta ee OH ee kooxaha hydroxyl43. Natiijooyinkani waxay la jaan qaadayaan muuqaalka XPS ee Jaantusyada 4b, halkaas oo kooxaha shaqada ee WO ay ku bixin karaan goobo firfircoon oo loogu talagalay falcelinta VO2+/VO2+.
Falanqaynta FTIR ee HWO iyo HWO-50% C76 (a), waxay muujisay kooxo shaqeynaya iyo cabbiraadaha xagasha xiriirka (b, c).
Kooxda OH waxay sidoo kale kicin kartaa falcelinta VO2+/VO2+, iyadoo kordhinaysa hydrophilicity-ga elektroodka, taasoo kor u qaadaysa heerka faafinta iyo wareejinta elektroodka. Sida la muujiyay, muunadda HWO-50% C76 waxay muujinaysaa meel sare oo dheeraad ah oo loogu talagalay C76. Meelaha ugu sarreeya ee ~2905, 2375, 1705, 1607, iyo 1445 cm3 waxaa loo qoondeyn karaa gariirka fidinta CH, O=C=O, C=O, C=C, iyo CO, siday u kala horreeyaan. Waa la ogyahay in kooxaha shaqeynaya ee oksijiinta C=O iyo CO ay u adeegi karaan xarumo firfircoon oo loogu talagalay falcelinta redox ee vanadium. Si loo tijaabiyo oo loo barbardhigo qoyaanka labada elektroodh, cabbiraadaha xagasha xiriirka ayaa la qaaday sida lagu muujiyey Jaantuska 5b,c. Elektroodka HWO isla markiiba wuxuu nuugaa dhibcaha biyaha, taasoo muujinaysa superhydrophilicity sababtoo ah kooxaha shaqeynaya ee OH ee la heli karo. HWO-50% C76 waa hydrophobic badan, xagasha xiriirka oo qiyaastii ah 135° 10 ilbiriqsi ka dib. Si kastaba ha ahaatee, cabbiraadaha elektiroonigga ah, elektroodka HWO-50%C76 wuxuu gebi ahaanba qoyanaaday wax ka yar daqiiqad gudaheed. Cabbiraadaha qoyaanka waxay la jaan qaadayaan natiijooyinka XPS iyo FTIR, taasoo muujinaysa in kooxo OH ah oo badan oo ku yaal dusha sare ee HWO ay ka dhigayaan mid aad u biyo-baxsan.
Falcelinta VO2+/VO2+ ee nanocomposites-ka HWO iyo HWO-C76 ayaa la tijaabiyay waxaana la filayay in HWO ay xakamayso isbeddelka koloriin ee falgalka VO2+/VO2+ ee aashitada isku dhafan, C76-na waxay sii kicin doontaa falgalka redox ee VO2+/VO2+ ee la rabo. %, 30%, iyo 50% C76 ee joojinta HWO iyo CCC oo lagu shubay elektroodhada iyadoo wadarta guud ee culaysku yahay qiyaastii 2 mg/cm2.
Sida ku cad jaantuska 6, kinetics-ka falcelinta VO2+/VO2+ ee dusha sare ee elektroodka waxaa lagu baaray CV oo ku jira elektrooti isku dhafan oo aashito leh. Hirarka waxaa lagu muujiyay I/Ipa si loo fududeeyo isbarbardhigga ΔEp iyo Ipa/Ipc ee kaaliyayaasha kala duwan si toos ah garaafka. Xogta cutubka aagga hadda jira waxaa lagu muujiyay Jaantuska 2S. Jaantuska 6a wuxuu muujinayaa in HWO uu si yar u kordhiyo heerka wareejinta elektroodka ee falcelinta redox ee VO2+/VO2+ ee dusha sare ee elektroodka isla markaana uu joojiyo falcelinta horumarka koloriin-ka dulinka ah. Si kastaba ha ahaatee, C76 si weyn ayuu u kordhiyaa heerka wareejinta elektroodka wuxuuna kiciyaa falcelinta horumarka koloriinka. Sidaa darteed, isku-darka si sax ah loo sameeyay ee HWO iyo C76 ayaa la filayaa inuu yeesho dhaqdhaqaaqa ugu fiican iyo awoodda ugu weyn ee lagu joojin karo falcelinta horumarka koloriinka. Waxaa la ogaaday in ka dib markii la kordhiyay nuxurka C76, dhaqdhaqaaqa elektroodka ee elektroodka uu soo hagaagay, sida lagu caddeeyay hoos u dhac ku yimid ΔEp iyo kororka saamiga Ipa/Ipc (Jadwalka S3). Tan waxaa sidoo kale xaqiijiyay qiimayaasha RCT ee laga soo saaray sawirka Nyquist ee Jaantuska 6d (Jadwalka S3), kuwaas oo la ogaaday inay hoos u dhaceen iyadoo la kordhinayo tirada C76. Natiijooyinkani waxay sidoo kale la jaan qaadayaan daraasadda Li, taas oo ku darista kaarboon mesoporous ah ee mesoporous WO3 ay muujisay dhaqdhaqaaqa wareejinta dallacaadda oo wanaagsanaaday VO2+/VO2+35. Tani waxay muujinaysaa in falcelinta tooska ah ay ku xirnaan karto wax badan oo ku saabsan gudbinta elektroodka (C=C bond) 18, 24, 35, 36, 37. Tani waxay sidoo kale sabab u noqon kartaa isbeddel ku yimid qaab-dhismeedka isku-dubaridka ee u dhexeeya [VO(H2O)5]2+ iyo [VO2(H2O)4]+, C76 waxay yareysaa danabka xad-dhaafka ah ee falcelinta iyadoo la dhimayo tamarta unugyada. Si kastaba ha ahaatee, tani waxaa laga yaabaa inaysan suurtogal ahayn elektroodhada HWO.
(a) Dhaqanka wareegga ah ee voltammetric (ν = 5 mV/s) ee falgalka VO2+/VO2+ ee isku-darka UCC iyo HWO-C76 oo leh saamiyo HWO:C76 oo kala duwan oo ku jira 0.1 M VOSO4/1 M H2SO4 + 1 M HCl elektrolyt. (b) Randles-Sevchik iyo (c) Habka Nicholson VO2+/VO2+ si loo qiimeeyo waxtarka faafinta iyo helitaanka qiimayaasha k0(d).
Ma aha oo kaliya in HWO-50% C76 ay muujisay ku dhawaad ​​​​dhaqdhaqaaq koronto oo la mid ah C76 ee falcelinta VO2+/VO2+, laakiin, si ka sii xiiso badan, waxay sidoo kale xakamaysay horumarka koloriin marka la barbar dhigo C76, sida ka muuqata Jaantuska 6a, waxayna sidoo kale muujisay wareeg yar oo ku yaal Jaantuska 6d (RCT hoose). C76 waxay muujisay Ipa/Ipc oo ka sarreeya HWO-50% C76 (Jadwalka S3), ma aha sababtoo ah dib-u-noqoshada falcelinta oo la hagaajiyay, laakiin sababtoo ah isku-darka ugu sarreeya ee falcelinta dhimista koloriin ee SHE ee 1.2 V. Waxqabadka ugu wanaagsan ee HWO- 50% C76 waxaa loo aanaynayaa saameynta isku-dhafka ah ee u dhaxaysa C76-ka si xun u dallacaya ee aadka u gudbiya iyo shaqada qoyaanka sare iyo shaqada kicinta W-OH ee HWO. Sii deynta koloriin oo yar ayaa hagaajin doonta hufnaanta dallacaadda ee unugga oo dhan, halka kinetics-ka la hagaajiyay ay hagaajin doonaan hufnaanta danabka unugyada oo dhan.
Sida ku cad isleegga S1, falgalka wareejinta elektarooniga ee quasi-reversible (oo gaabis ah) oo lagu xakameeyo faafinta, hadda ugu sarreysa (IP) waxay ku xiran tahay tirada elektaroonada (n), aagga elektaroonada (A), isku-dhafka faafinta (D), tirada isku-dhafka wareejinta elektaroonada (α) iyo xawaaraha iskaanka (ν). Si loo barto dhaqanka xakamaynta faafinta ee walxaha la tijaabiyay, xiriirka ka dhexeeya IP iyo ν1/2 ayaa la sawiray oo lagu soo bandhigay Jaantuska 6b. Maadaama dhammaan agabku ay muujinayaan xiriir toosan, falcelinta waxaa lagu xakameeyaa faafinta. Maadaama falcelinta VO2+/VO2+ ay tahay mid quasi-reversible ah, jiirada xariiqda waxay ku xiran tahay isku-dhafka faafinta iyo qiimaha α (isle'egta S1). Maadaama isku-dhafka faafinta uu yahay mid joogto ah (≈ 4 × 10–6 cm2/s)52, farqiga u dhexeeya jiirada xariiqda ayaa si toos ah u muujinaya qiimayaal kala duwan oo α ah, sidaas darteedna heerka wareejinta elektarooniga ee dusha sare ee elektiroonigga, kaas oo lagu muujiyay C76 iyo HWO -50% C76 jiirada ugu sarreysa (heerka wareejinta elektarooniga ugu sarreeya).
Jaranjarooyinka Warburg (W) ee lagu xisaabiyay mawjadaha hoose ee lagu muujiyay Shaxda S3 (Jaantuska 6d) waxay leeyihiin qiimo u dhow 1 dhammaan agabka, taasoo muujinaysa faafin qumman oo noocyada redox ah iyo xaqiijinta dhaqanka toosan ee IP marka la barbar dhigo ν1/2. CV waa la cabbiraa. HWO-50% C76, jiirada Warburg waxay ka leexataa 1 ilaa 1.32, taasoo muujinaysa ma aha oo kaliya faafinta nus-aan xadidnayn ee reagent-ka (VO2+), laakiin sidoo kale waxay gacan ka geysan kartaa dhaqanka lakabka khafiifka ah ee dhaqanka faafinta sababtoo ah daloolka elektiroonigga.
Si loo sii falanqeeyo dib-u-noqoshada (heerka wareejinta elektarooniga) ee falgalka redox-ka VO2+/VO2+, habka falgalka Nicholson ee isku-dhafan ayaa sidoo kale loo isticmaalay in lagu go'aamiyo heerka caadiga ah ee joogtada ah ee k041.42. Tan waxaa lagu sameeyaa iyadoo la adeegsanayo isla'egta S2 si loo dhiso halbeegga kinetic-ga aan cabbir lahayn ee Ψ, kaas oo ah shaqo ΔEp ah, oo ah shaqo ν-1/2 ah. Shaxda S4 waxay muujinaysaa qiimayaasha Ψ ee laga helay walxo elektroodh kasta. Natiijooyinka (Jaantuska 6c) waxaa loo sawiray si loo helo k0 × 104 cm/s laga bilaabo jiirada sawir kasta iyadoo la adeegsanayo Isle'egta S3 (oo ku qoran safka dhinaciisa oo lagu soo bandhigay Shaxda S4). HWO-50% C76 waxaa la ogaaday inay leedahay jiirada ugu sarreysa (Jaantuska 6c), sidaas darteed qiimaha ugu badan ee k0 waa 2.47 × 10–4 cm/s. Taas macnaheedu waa in elektroodkani uu gaaro kinetics-ka ugu dhaqsaha badan, kaas oo la jaanqaadaya natiijooyinka CV iyo EIS ee Jaantuska 6a iyo d iyo Shaxda S3. Intaa waxaa dheer, qiimaha k0 waxaa sidoo kale laga helay sawirka Nyquist (Jaantuska 6d) ee Isle'egta S4 iyadoo la adeegsanayo qiimaha RCT (Jadwalka S3). Natiijooyinkan k0 ee ka imanaya EIS waxaa lagu soo koobay Shaxda S4 waxayna sidoo kale muujinayaan in HWO-50% C76 ay muujinayso heerka ugu sarreeya ee wareejinta elektaroonigga sababtoo ah saameynta isku-dhafka ah. Inkasta oo qiimayaasha k0 ay kala duwan yihiin sababtoo ah asalka kala duwan ee hab kasta, haddana waxay muujinayaan isku mid ah baaxadda waxayna muujinayaan isku-dheellitirnaan.
Si aad si buuxda u fahamto kinetics-ka aadka u fiican ee la helay, waxaa muhiim ah in la barbar dhigo walxaha elektroodka ugu fiican elektroodka UCC iyo TCC ee aan dahaarka lahayn. Falcelinta VO2+/VO2+, HWO-C76 ma muujin oo keliya ΔEp ugu hooseeya iyo dib u celin wanaagsan, laakiin sidoo kale si weyn ayuu u xakameeyay falgalka isbeddelka koloriinka dulinka ah marka loo eego TCC, sida lagu cabbiray hadda 1.45 V marka loo eego SHE (Jaantuska 7a). Marka laga hadlayo xasilloonida, waxaan u qaadannay in HWO-50% C76 uu ahaa mid jir ahaan deggan sababtoo ah kicinta waxaa lagu qasay xidhmo PVDF ah ka dibna lagu mariyey elektroodka maro kaarboon. HWO-50% C76 waxay muujisay isbeddel ugu sarreeya oo ah 44 mV (heerka burburka 0.29 mV/wareeg) ka dib 150 wareeg marka la barbar dhigo 50 mV ee UCC (Jaantuska 7b). Tani waxaa laga yaabaa inaysan ahayn farqi weyn, laakiin kinetics-ka elektroodka UCC waa mid aad u gaabis ah oo hoos u dhaca marka la socdo wareegga, gaar ahaan falcelinta gadaal. In kasta oo dib-u-noqoshada TCC ay aad uga fiican tahay tan UCC, TCC waxaa la ogaaday inay leedahay isbeddel weyn oo ah 73 mV ka dib 150 wareeg, taasoo laga yaabo inay sabab u tahay xaddiga badan ee koloriin ee lagu sameeyay dusha sare. si uu kiciyuhu si fiican ugu dhego dusha sare ee elektroodka. Sida laga arki karo dhammaan elektroodhada la tijaabiyay, xitaa elektroodhada aan lahayn kiciyeyaasha la taageeray waxay muujiyeen heerar kala duwan oo xasillooni darro wareeg ah, taasoo soo jeedinaysa in isbeddelka kala-soocidda ugu sarreysa inta lagu jiro wareegga ay sabab u tahay joojinta walxaha ay sababaan isbeddellada kiimikada halkii laga kala sooci lahaa kiciyeyaasha. Intaa waxaa dheer, haddii xaddi badan oo walxaha kiciyeyaasha ah laga sooco dusha sare ee elektroodka, tani waxay keeni doontaa koror weyn oo ku yimaada kala-soocidda ugu sarreysa (ma aha oo kaliya 44 mV), maadaama substrate-ka (UCC) uu yahay mid aan firfircoonayn falcelinta redox ee VO2+/VO2+.
Isbarbardhigga CV-ga ee walaxda elektroodka ugu fiican marka la barbar dhigo UCC (a) iyo xasilloonida falcelinta redox ee VO2+/VO2+ (b). ν = 5 mV/s dhammaan CV-yada ku jira 0.1 M VOSO4/1 M H2SO4 + 1 M elektroodka HCl.
Si loo kordhiyo soo jiidashada dhaqaale ee tignoolajiyada VRFB, ballaarinta iyo fahamka kinetics-ka falcelinta redox ee vanadium waa lama huraan si loo gaaro hufnaan tamar sare leh. Waxyaabaha isku dhafan ee HWO-C76 ayaa la diyaariyey waxaana la darsay saameyntooda electrocatalytic-ga ee falgalka VO2+/VO2+. HWO waxay muujisay kor u qaadis yar oo kinetic ah oo ku jirta electrolytes-ka aashitada isku dhafan laakiin si weyn ayay u xakamaysay horumarka chlorine-ka. Saamiyada kala duwan ee HWO:C76 ayaa loo isticmaalay in lagu sii wanaajiyo kinetics-ka elektroodhada ku salaysan HWO. Kordhinta C76 ilaa HWO waxay hagaajinaysaa kinetics-ka wareejinta elektarooniga ee falgalka VO2+/VO2+ ee elektroodka la beddelay, kaas oo HWO-50% C76 uu yahay walaxda ugu fiican sababtoo ah waxay yareysaa iska caabbinta wareejinta dallacaadda waxayna sii xakameysaa koloriin marka la barbar dhigo dhigaalka C76 iyo TCC. Tani waxay sabab u tahay saameynta isku-dhafka ah ee u dhaxaysa isku-dhafka C=C sp2, OH iyo kooxaha shaqeynaya ee W-OH. Heerka burburka ka dib wareegyada soo noqnoqda ee HWO-50% C76 waxaa la ogaaday inuu yahay 0.29 mV/wareeg, halka heerka burburka ee UCC iyo TCC uu yahay 0.33 mV/wareeg iyo 0.49 mV/wareeg, siday u kala horreeyaan, taasoo ka dhigaysa mid aad u deggan. electrolytes-ka aashitada isku dhafan. Natiijooyinka la soo bandhigay waxay si guul leh u aqoonsadeen agabka elektroodka waxqabadka sare leh ee falcelinta VO2+/VO2+ oo leh kinetics degdeg ah iyo xasillooni sare. Tani waxay kordhin doontaa danabka wax soo saarka, taasoo kordhin doonta hufnaanta tamarta ee VRFB, sidaas darteedna waxay yareyn doontaa kharashka ganacsigeeda mustaqbalka.
Xogta xogta ee la isticmaalay iyo/ama lagu falanqeeyay daraasadda hadda jirta waxaa laga heli karaa qorayaasha ku habboon marka la codsado.
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