I-Wet Chemical Synthesis Nezithasiselo Zokulawula I-Nickel Cobaltate Surface Area yokutholwa kweGlucose

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Siphenye umthelela wendawo ethile endaweni ye-electrochemical ye-NiCo2O4 (NCO) ukuze kutholwe ushukela.Ama-nanomaterials e-NCO anendawo ethile elawulwayo akhiqizwe ukuhlanganiswa kwe-hydrothermal enezithasiselo, kanye nama-nanostructures azihlanganisayo ane-hedgehog, inaliti kaphayini, i-tremella nembali efana ne-morphology nayo iye yakhiqizwa.Intsha yale ndlela ilele ekulawuleni okuhlelekile kwendlela yokusabela kwamakhemikhali ngokwengeza izithasiselo ezihlukahlukene ngesikhathi sokuhlanganiswa, okuholela ekwakhekeni okuzenzakalelayo kwama-morphologies ahlukahlukene ngaphandle komehluko ekwakhekeni kwekristalu kanye nesimo samakhemikhali sezakhi ezikhona.Lokhu kulawulwa kwe-morphological ye-NCO nanomaterials kuholela ezinguqukweni ezibalulekile ekusebenzeni kwe-electrochemical kokutholwa kweglucose.Ngokuhambisana nokuhlukaniswa kwezinto, kwaxoxwa ngobudlelwano phakathi kwendawo ethile kanye nokusebenza kwe-electrochemical ukuze kutholwe i-glucose.Lo msebenzi ungase unikeze ukuqonda kwesayensi ekulungiseni kwendawo engaphezulu kwama-nanostructures anquma ukusebenza kwawo ekusetshenzisweni okungase kube khona kuma-biosensors eglucose.
Amazinga kashukela wegazi ahlinzeka ngolwazi olubalulekile mayelana nesimo se-metabolic kanye nesokuphila komzimba1,2.Isibonelo, amazinga eglucose engavamile emzimbeni angaba inkomba ebalulekile yezinkinga zempilo ezingathi sína, kuhlanganise nesifo sikashukela, isifo senhliziyo nemithambo yegazi, nokukhuluphala ngokweqile3,4,5.Ngakho-ke, ukuqapha njalo amazinga kashukela egazini kubaluleke kakhulu ekugcineni impilo enhle.Nakuba izinhlobo ezihlukahlukene zezinzwa ze-glucose ezisebenzisa ukutholwa kwe-physicochemical ziye zabikwa, ukuzwela okuphansi kanye nezikhathi zokuphendula kancane zihlala ziyizithiyo ezinhlelweni eziqhubekayo zokuqapha i-glucose6,7,8.Ngaphezu kwalokho, izinzwa ze-glucose ze-electrochemical ezithandwayo njengamanje ezisekelwe ekuphenduleni kwe-enzymatic zisenemikhawulo ethile naphezu kwezinzuzo zazo zokusabela okusheshayo, ukuzwela okuphezulu kanye nezinqubo zokwenziwa ezilula kakhulu9,10.Ngakho-ke, izinhlobo ezihlukahlukene zezinzwa ze-electrochemical ezingezona i-enzymatic ziye zacwaningwa kabanzi ukuze kuvinjelwe ukuchithwa kwe-enzyme ngenkathi kugcinwa izinzuzo ze-electrochemical biosensors9,11,12,13.
I-Transition metal compounds (i-TMCs) inomsebenzi ophezulu ngokwanele we-catalytic ngokuphathelene ne-glucose, enweba ububanzi bokusebenza kwayo kuzinzwa ze-electrochemical glucose13,14,15.Kuze kube manje, imiklamo ehlukahlukene enengqondo nezindlela ezilula zokwenziwa kwe-TMS ziye zahlongozwa ukuze kuthuthukiswe ukuzwela, ukukhetha, nokuzinza kwe-electrochemical kokutholwa kwe-glucose16,17,18.Isibonelo, ama-oxide ensimbi eguquguqukayo angacacile afana ne-copper oxide (CuO)11,19, i-zinc oxide (ZnO)20, i-nickel oxide (NiO)21,22, i-cobalt oxide (Co3O4) 23,24 ne-cerium oxide (CeO2) 25 i-electrochemically isebenza ngokuphathelene ne-glucose.Intuthuko yakamuva kuma-oxide ensimbi kanambambili njenge-nickel cobaltate (NiCo2O4) yokutholwa kwe-glucose ibonise imiphumela eyengeziwe ye-synergistic ngokuya ngomsebenzi owandayo kagesi26,27,28,29,30.Ikakhulukazi, ukubunjwa okunembile kanye nokulawulwa kwe-morphology ukwakha i-TMS enezinhlobonhlobo ze-nanostructures kungakhuphula ngokuphumelelayo ukuzwela kokutholwa ngenxa yendawo yabo enkulu, ngakho-ke kunconywa kakhulu ukuthuthukisa i-TMS elawulwa yi-morphology ukuze kutholakale ukutholakala kwe-glucose okuthuthukisiwe20,25,30,31,32, 33.34, 35.
Lapha sibika ama-NiCo2O4 (NCO) nanomatadium ane-morphology ehlukene yokutholwa kwe-glucose.I-NCO nanomaterials itholakala ngendlela elula ye-hydrothermal isebenzisa izithasiselo ezihlukahlukene, izithasiselo zamakhemikhali zingenye yezinto ezibalulekile ekuzihlanganiseni kwe-nanostructures ye-morphology ehlukahlukene.Siphenye ngokuhlelekile umthelela wama-NCO anama-morphology ahlukene ekusebenzeni kwawo kwe-electrochemical ukuze kutholwe i-glucose, okuhlanganisa ukuzwela, ukukhetha, umkhawulo wokutholwa ophansi, nokuzinza kwesikhathi eside.
Sihlanganise i-NCO nanomaterials (efushanisiwe i-UNCO, i-PNCO, i-TNCO ne-FNCO ngokulandelanayo) ngama-microstructures afana nama-sea urchin, izinaliti zikaphayini, i-tremella nezimbali.Umfanekiso 1 ubonisa i-morphology ehlukene ye-UNCO, i-PNCO, i-TNCO, ne-FNCO.Izithombe ze-SEM nezithombe ze-EDS zibonise ukuthi i-Ni, Co, kanye ne-O zasatshalaliswa ngokulinganayo kuma-nanomaterials e-NCO, njengoba kuboniswe kuMfanekiso 1 no-2. I-S1 ne-S2, ngokulandelana.Emkhiwaneni.I-2a,b ibonisa izithombe ezimele ze-TEM ze-NCO nanomaterials ezine-morphology ehlukile.I-UNCO iyi-microsphere ezihlanganisayo (ububanzi: ~5 µm) ehlanganiswe nama-nanowires ane-NCO nanoparticles (isilinganiso sosayizi wezinhlayiyana: 20 nm).Lesi sakhiwo esincane esiyingqayizivele kulindeleke ukuthi sinikeze indawo enkulu engaphezulu ukuze kube lula ukusakazeka kwe-electrolyte kanye nokuthuthwa kwama-electron.Ukwengezwa kwe-NH4F ne-urea ngesikhathi sokuhlanganiswa kubangele ukuqina kwe-acicular microstructure (PNCO) engu-3 µm ubude no-60 nm ububanzi, eyakhiwe ngama-nanoparticles amakhulu.Ukwengezwa kwe-HMT esikhundleni se-NH4F kubangela i-tremello-like morphology (TNCO) enama-nanosheet ashwabene.Ukwethulwa kwe-NH4F ne-HMT ngesikhathi sokuhlanganiswa kuholela ekuhlanganisweni kwama-nanosheet aminyene aseduze, okuholela ku-morphology efana nembali (FNCO).Isithombe se-HREM (I-Fig. 2c) sibonisa amabhendi okugaya ahlukile anezikhala ze-interplanar ezingu-0.473, 0.278, 0.50, kanye no-0.237 nm, okuhambisana ne-(111), (220), (311), kanye (222) izindiza ze-NiCo2O4, s 27 .Iphethini yendawo ekhethiwe ye-electron diffraction (SAED) ye-NCO nanomaterials (ifakwe ku-Fig. 2b) iphinde yaqinisekisa imvelo ye-polycrystalline ye-NiCo2O4.Imiphumela ye-high-angle annular imaging dark (HAADF) kanye nemephu ye-EDS ibonisa ukuthi zonke izici zisakazwa ngokulinganayo ku-NCO nanomaterial, njengoba kuboniswe ku-Fig. 2d.
Umfanekiso ohleliwe wenqubo yokwakhiwa kwe-NiCo2O4 nanostructures ene-morphology elawulwayo.I-Schematics nezithombe ze-SEM zama-nanostructures ahlukahlukene nazo ziyaboniswa.
Ukucaciswa kwe-morphological kanye nesakhiwo se-NCO nanomaterials: (a) Isithombe se-TEM, (b) Isithombe se-TEM kanye nephethini ye-SAED, (c) isithombe se-HRTEM esixazululwe ngokusanhlamvu kanye nemifanekiso ehambisanayo ye-HADDF ye-Ni, Co, ne-O in (d) nanomaterials ye-NCO..
Amaphethini we-X-ray diffraction we-NCO nanomaterials we-morphology ehlukahlukene aboniswa ku-Fig.3a.Ukuphakama kwe-diffraction ku-18.9, 31.1, 36.6, 44.6, 59.1 kanye no-64.9° kubonisa izindiza (111), (220), (311), (400), (511) kanye (440) ne-NiCo2O4, ngokulandelana, ezine-cubic isakhiwo somgogodla (JCPDS No. 20-0781) 36. I-spectra ye-FT-IR ye-NCO nanomaterials ikhonjiswe ku-Fig.3b.Amabhendi amabili okudlidliza aqinile esifundeni phakathi kuka-555 no-669 cm–1 ahambisana nomoya-mpilo we-metallic (Ni no-Co) othathwe endaweni ye-tetrahedral kanye ne-octahedral ye-NiCo2O437 spinel, ngokulandelana.Ukuze uqonde kangcono izakhiwo ze-NCO nanomaterials, i-Raman spectra itholwe njengoba kuboniswe kumfanekiso 3c.Iziqongo ezine ezibonwe ku-180, 459, 503, kanye ne-642 cm-1 zihambisana nezindlela ze-Raman F2g, E2g, F2g, kanye ne-A1g ye-NiCo2O4 spinel, ngokulandelanayo.Izilinganiso ze-XPS zenziwe ukuze kutholwe isimo samakhemikhali esingaphezulu sezinto ku-NCO nanomatadium.Emkhiwaneni.I-3d ibonisa i-XPS spectrum ye-UNCO.I-spectrum ye-Ni 2p ineziqongo ezimbili eziyinhloko ezitholakala kumandla abophayo we-854.8 kanye ne-872.3 eV, ehambisana ne-Ni 2p3/2 ne-Ni 2p1/2, kanye namasathelayithi amabili adlidlizayo ku-860.6 kanye no-879.1 eV, ngokulandelana.Lokhu kukhombisa ubukhona bezifunda ze-Ni2+ ne-Ni3+ e-NCO.Iziqongo eziseduze kuka-855.9 kanye no-873.4 eV eze-Ni3+, kanti ukuphakama okungaba ngu-854.2 kanye no-871.6 eV eze-Ni2+.Ngokufanayo, i-Co2p spectrum yama-spin-orbit doublet embula izici eziphakeme ze-Co2+ ne-Co3+ ku-780.4 (Co 2p3/2) kanye ne-795.7 eV (Co 2p1/2).Ukuphakama okungu-796.0 no-780.3 eV kuhambelana ne-Co2+, futhi ukuphakama okungu-794.4 no-779.3 eV kuhambisana ne-Co3+.Kumele kuqashelwe ukuthi isimo se-polyvalent se-ion yensimbi (Ni2 +/ Ni3 + ne-Co2 +/ Co3 +) ku-NiCo2O4 sikhuthaza ukwanda komsebenzi we-electrochemical37,38.I-spectra ye-Ni2p ne-Co2p ye-UNCO, i-PNCO, i-TNCO, ne-FNCO ibonise imiphumela efanayo, njengoba kuboniswe kumfanekiso.I-S3.Ukwengeza, i-spectra ye-O1s yawo wonke ama-NCO nanomaterials (I-Fig. S4) ibonise iziqongo ezimbili ku-592.4 kanye no-531.2 eV, ezazihlotshaniswa ne-metal-oxygen ne-oxygen bond evamile emaqenjini e-hydroxyl endaweni ye-NCO, ngokulandelana39.Nakuba izakhiwo ze-NCO nanomatadium zifana, umehluko we-morphological ezithasiselweni uphakamisa ukuthi isithasiselo ngasinye singabamba iqhaza ngendlela ehlukile ekuphenduleni kwamakhemikhali ukuze kwakhe i-NCO.Lokhu kulawula i-nucleation evumayo ngamandla nezinyathelo zokukhula okusanhlamvu, ngaleyo ndlela ilawula usayizi wezinhlayiyana kanye nezinga le-agglomeration.Ngakho-ke, ukulawulwa kwemingcele yenqubo ehlukahlukene, okuhlanganisa izithasiselo, isikhathi sokuphendula, kanye nezinga lokushisa ngesikhathi sokuhlanganiswa, kungasetshenziswa ukuklama i-microstructure futhi kuthuthukiswe ukusebenza kwe-electrochemical ye-NCO nanomaterials ukuze kutholwe i-glucose.
(a) Amaphethini e-X-ray diffraction, (b) FTIR kanye (c) ne-Raman spectra ye-NCO nanomaterials, (d) i-XPS spectra ye-Ni 2p ne-Co 2p evela ku-UNCO.
I-morphology ye-NCO nanomaterials eguquliwe ihlobene eduze nokwakheka kwezigaba zokuqala ezitholwe ezithasiselweni ezihlukahlukene ezivezwe kuMfanekiso S5.Ngaphezu kwalokho, i-X-ray kanye ne-Raman spectra yamasampula asanda kulungiselelwa (Izibalo S6 kanye ne-S7a) ibonise ukuthi ukubandakanyeka kwezithasiselo zamakhemikhali ezahlukene kubangele umehluko we-crystallographic: I-Ni ne-Co carbonate hydroxides yayibhekwa ikakhulukazi kuma-urchins olwandle kanye nesakhiwo senalithi sikaphayini, kuyilapho njenge izakhiwo ngendlela ye-tremella nembali zibonisa ukuba khona kwe-nickel ne-cobalt hydroxides.I-spectra ye-FT-IR ne-XPS yamasampuli alungisiwe aboniswa ku-Figure 1 kanye no-2. I-S7b-S9 iphinde inikeze ubufakazi obucacile bomehluko oshiwo ngenhla we-crystallographic.Kusukela ezintweni ezibonakalayo zamasampula alungisiwe, kuyacaca ukuthi izithasiselo zihileleke ekuphenduleni kwe-hydrothermal futhi zinikeze izindlela zokusabela ezihlukene zokuthola izigaba zokuqala nge-morphologies ehlukene40,41,42.Ukuzihlanganisa kwama-morphologies ahlukene, okuhlanganisa ama-nanowires anohlangothi olulodwa (1D) kanye nama-nanosheet anezinhlangothi ezimbili (2D), kuchazwa isimo samakhemikhali esihlukene sezigaba zokuqala (i-Ni ne-Co ions, kanye namaqembu asebenzayo), kulandelwa ukukhula kwe-crystal42, 43, 44, 45, 46, 47. Ngesikhathi sokucubungula kwe-post-thermal, izigaba ezihlukahlukene zokuqala ziguqulwa zibe yi-NCO spinel ngenkathi zigcina i-morphology yazo eyingqayizivele, njengoba kuboniswe ku-Figure 1 no-2. 2 no-3a.
Umehluko we-morphological ku-NCO nanomatadium ungase ube nomthelela endaweni esebenza nge-electrochemically ukuze kutholwe i-glucose, ngaleyo ndlela kunqunywe izici eziphelele ze-electrochemical zenzwa ye-glucose.I-N2 BET adsorption-desorption isotherm isetshenziselwe ukulinganisa usayizi wezimbotshana nendawo ethile ye-NCO nanomaterials.Emkhiwaneni.4 ibonisa ama-BET ama-isotherm ama-NCO nanomaterials ahlukahlukene.Indawo ethize ye-BET ye-UNCO, i-PNCO, i-TNCO ne-FNCO ilinganiselwa ku-45.303, 43.304, 38.861 kanye no-27.260 m2/g, ngokulandelana.I-UNCO inendawo ephakeme kakhulu ye-BET (45.303 m2 g-1) kanye nevolumu enkulu yembotshana (0.2849 cm3 g-1), futhi ukusabalalisa kosayizi wembotshana kuncane.Imiphumela ye-BET ye-NCO nanomatadium ikhonjiswe kuThebula 1. Amajika e-N2 adsorption-desorption ayefana kakhulu nohlobo lwe-IV isothermal hysteresis loops, okubonisa ukuthi wonke amasampula anesakhiwo se-mesoporous48.Ama-UNCO ama-Mesoporous anendawo ephakeme kakhulu kanye nevolumu yembotshana ephakeme kakhulu kulindeleke ukuthi ahlinzeke ngezindawo eziningi ezisebenzayo zokusabela kwe-redox, okuholela ekusebenzeni okuthuthukisiwe kwe-electrochemical.
Imiphumela yeBET ye (a) UNCO, (b) PNCO, (c) TNCO, kanye (d) FNCO.Isingeniso sibonisa ukusatshalaliswa kosayizi wembotshana okuhambisanayo.
Ukusabela kwe-electrochemical redox kwe-NCO nanomatadium ezinama-morphology ahlukahlukene ukuze kutholwe i-glucose kuye kwahlolwa kusetshenziswa izilinganiso ze-CV.Emkhiwaneni.I-5 ibonisa amajika e-CV we-NCO nanomaterials ku-0.1 M NaOH alkaline electrolyte eno-5 mM glucose nangenayo ngesilinganiso sokuskena esingu-50 mVs-1.Uma i-glucose ingekho, iziqongo ze-redox zibonwe ku-0.50 no-0.35 V, okuhambisana ne-oxidation ehlotshaniswa ne-M-O (M: Ni2+, Co2+) kanye ne-M *-O-OH (M*: Ni3+, Co3+).usebenzisa i-OH anion.Ngemva kokwengezwa kwe-glucose engu-5 mM, ukusabela kwe-redox ebusweni be-nanomaterials ye-NCO kwanda kakhulu, okungase kube ngenxa ye-oxidation ye-glucose ku-gluconolactone.Umfanekiso we-S10 ubonisa ukuphakama kwe-redox yamanje ngamanani wokuskena we-5–100 mV s-1 kusixazululo esingu-0.1 M NaOH.Kuyacaca ukuthi i-peak redox yamanje ikhuphuka ngokunyuka kwezinga lokuskena, okubonisa ukuthi i-NCO nanomaterials inokusabalalisa okufanayo okulawulwa kokuziphatha kwe-electrochemical50,51.Njengoba kuboniswe kumfanekiso we-S11, indawo ye-electrochemical surface (ECSA) ye-UNCO, PNCO, TNCO, ne-FNCO ilinganiselwa ku-2.15, 1.47, 1.2, kanye no-1.03 cm2, ngokulandelanayo.Lokhu kuphakamisa ukuthi i-UNCO ilusizo kunqubo ye-electrocatalytic, yenza kube lula ukutholwa kweglucose.
Amajika e-CV (a) UNCO, (b) PNCO, (c) TNCO, kanye (d) nama-electrodes e-FNCO angenayo i-glucose futhi angezwe ngo-5 mM glucose ngesilinganiso sokuskena esingu-50 mVs-1.
Ukusebenza kwe-electrochemical kwe-NCO nanomatadium ukuze kutholwe i-glucose kuye kwaphenywa futhi imiphumela iboniswa ku-Fig. 6. Ukuzwela kwe-glucose kwanqunywa indlela ye-CA ngokungeza kancane kancane ukugxila okuhlukahlukene kweglucose (0.01–6 mM) kusisombululo esingu-0.1 M NaOH esingu-0.5 V ngesikhawu sama-60 s.Njengoba kuboniswe emkhiwaneni.I-6a–d, i-NCO nanomatadium ikhombisa ukuzwela okuhlukene kusukela ku-84.72 kuya ku-116.33 µA mM-1 cm-2 nama-coefficients aphezulu wokuxhumanisa (R2) ukusuka ku-0.99 kuya ku-0.993.Ijika lokulinganisa phakathi kokugxiliswa kweglucose kanye nokusabela kwamanje kwe-NCO nanomaterials kuboniswa kufig.I-S12.Imikhawulo ebaliwe yokutholwa (LOD) ye-NCO nanomatadium ibikububanzi obungu-0.0623–0.0783 µM.Ngokwemiphumela yokuhlolwa kwe-CA, i-UNCO ibonise ukuzwela okuphezulu kakhulu (116.33 μA mM-1 cm-2) ebangeni elibanzi lokutholwa.Lokhu kungachazwa ngendlela eyingqayizivele efana ne-sea urchin-like morphology, ehlanganisa isakhiwo se-mesoporous esinendawo enkulu ethile ehlinzeka ngezindawo eziningi ezisebenzayo zezinhlobo ze-glucose.Ukusebenza kwe-electrochemical kwe-NCO nanomatadium okwethulwa kuThebula S1 kuqinisekisa ukusebenza okuhle kakhulu kokutholwa kwe-electrochemical glucose kwe-NCO nanomatadium okulungiselelwe kulolu cwaningo.
Izimpendulo ze-CA zama-electrodes e-UNCO (a), PNCO (b), TNCO (c), kanye ne-FNCO (d) aneglucose engezwe kusisombululo esingu-0.1 M NaOH ngo-0.50 V. Amasetha abonisa amajika okulinganisa ezimpendulo zamanje ze-NCO nanomaterials: (e ) Izimpendulo ze-KA ze-UNCO, (f) PNCO, (g) TNCO, kanye (h) ne-FNCO ngokungezwa kwesinyathelo ngesinyathelo kwe-glucose engu-1 mM kanye nezinto eziphazamisayo ezingu-0.1 mM (LA, DA, AA, ne-UA).
Ikhono lokulwa nokugxambukela lokutholwa kwe-glucose kungenye into ebalulekile ekutholeni okukhethiwe nokuzwela kwe-glucose ngokuphazamisa izinhlanganisela.Emkhiwaneni.I-6e–h ibonisa amandla okuvimbela ukuphazamiseka kwe-NCO nanomatadium kusixazululo esingu-0.1 M NaOH.Ama-molecule avamile aphazamisayo afana ne-LA, DA, AA ne-UA akhethiwe futhi engezwe ku-electrolyte.Ukusabela kwamanje kwe-NCO nanomatadium ku-glucose kuyabonakala.Kodwa-ke, impendulo yamanje ku-UA, DA, AA kanye ne-LA ayizange ishintshe, okusho ukuthi ama-NCO nanomaterials abonise ukukhetha okuhle kakhulu kokutholwa kwe-glucose kungakhathaliseki ukuhluka kwawo kwe-morphological.Umfanekiso S13 ubonisa ukuzinza kwama-NCO nanomatadium ahlolwe impendulo ye-CA ku-0.1 M NaOH, lapho i-glucose engu-1 mM yengezwe ku-electrolyte isikhathi eside (80,000 s).Izimpendulo zamanje ze-UNCO, i-PNCO, i-TNCO, ne-FNCO bezingu-98.6%, 97.5%, 98.4%, no-96.8%, ngokulandelana, zamanje zamanje ngokungezwa kwe-glucose engu-1 mM eyengeziwe ngemva kwe-80,000 s.Wonke ama-NCO nanomatadium abonisa ukusabela okuzinzile kwe-redox nezinhlobo ze-glucose isikhathi eside.Ikakhulukazi, isignali yamanje ye-UNCO ayizange igcine kuphela i-97.1% yamanje yayo yokuqala, kodwa futhi igcine izakhiwo zayo ze-morphology kanye nesibopho samakhemikhali ngemva kokuhlolwa kokuzinza kwemvelo yezinsuku ezingu-7 (Izibalo S14 kanye ne-S15a).Ngaphezu kwalokho, ukukhiqizwa kabusha nokukhiqizwa kabusha kwe-UNCO kwahlolwa njengoba kuboniswe ku-Fig. S15b, c.I-Relative Standard Deviation (RSD) ebaliwe yokuphindaphindeka nokuphindaphinda kwaba ngu-2.42% no-2.14%, ngokulandelana, okubonisa izinhlelo zokusebenza ezingase zibe khona njengenzwa yezinga lezimboni.Lokhu kukhombisa ukuzinza okuhle kakhulu kwesakhiwo namakhemikhali kwe-UNCO ngaphansi kwezimo ze-oxidizing zokutholwa kwe-glucose.
Kuyacaca ukuthi ukusebenza kwe-electrochemical kwe-NCO nanomaterials ekutholeni i-glucose ngokuyinhloko kuhlobene nezinzuzo zesakhiwo sesigaba sokuqala esilungiselelwe indlela ye-hydrothermal enezithasiselo (Fig. S16).Indawo ephezulu ye-UNCO inezindawo eziningi ezisebenza ngogesi kunezinye i-nanostructures, esiza ukuthuthukisa ukusabela kwe-redox phakathi kwezinto ezisebenzayo kanye nezinhlayiya ze-glucose.Isakhiwo se-mesoporous se-UNCO singadalula kalula amasayithi amaningi e-Ni and Co ku-electrolyte ukuze kutholakale i-glucose, okuholela ekuphenduleni okusheshayo kwe-electrochemical.Ama-nanowires anohlangothi olulodwa ku-UNCO angaqhubeka enyuse izinga lokusabalalisa ngokunikeza izindlela ezimfushane zokuthutha zama-ion nama-electron.Ngenxa yezici ezihlukile zesakhiwo ezishiwo ngenhla, ukusebenza kwe-electrochemical kwe-UNCO ekutholeni ushukela kuphakeme kunokwe-PNCO, TNCO, ne-FNCO.Lokhu kukhombisa ukuthi i-morphology ye-UNCO eyingqayizivele enendawo ephezulu kakhulu kanye nosayizi wezimbotshana inganikeza ukusebenza okuhle kakhulu kwe-electrochemical ukuze kutholwe ushukela.
Umthelela wendawo ethile ezicini ze-electrochemical ze-NCO nanomaterials wacwaningwa.Ama-NCO nanomatadium anendawo ethile ehlukile atholwe ngendlela elula ye-hydrothermal kanye nezithasiselo ezahlukahlukene.Izithasiselo ezihlukene ngesikhathi sokuhlanganiswa zingena ekuphenduleni kwamakhemikhali okuhlukene futhi zakha izigaba zokuqala ezihlukene.Lokhu kuye kwaholela ekuzihlanganiseni kwama-nanostructures ahlukahlukene ane-morphology efana ne-hedgehog, inaliti kaphayini, i-tremella, nembali.Ngemuva kokushisa okulandelanayo kuholela esimweni samakhemikhali esifanayo se-crystalline NCO nanomaterials enesakhiwo somgogodla ngenkathi igcina i-morphology yabo eyingqayizivele.Ngokuya ngendawo engaphezulu ye-morphology ehlukile, ukusebenza kwe-electrochemical kwe-NCO nanomaterials ekutholweni kweglucose kuye kwathuthukiswa kakhulu.Ikakhulukazi, ukuzwela kweglucose ye-NCO nanomaterials ene-sea urchin morphology ikhuphuke yafinyelela ku-116.33 µA mM-1 cm-2 nge-coefficient ephezulu yokuxhumanisa (R2) ka-0.99 kububanzi bomugqa obungu-0.01-6 mM.Lo msebenzi ungase unikeze isisekelo sesayensi sobunjiniyela be-morphological ukulungisa indawo ethile futhi uthuthukise ukusebenza kwe-electrochemical kwezinhlelo zokusebenza ze-non-enzymatic biosensor.
Ni(NO3)2 6H2O, Co(NO3)2 6H2O, urea, hexamethylenetetramine (HMT), ammonium fluoride (NH4F), sodium hydroxide (NaOH), d-(+)-glucose, lactic acid (LA), dopamine hydrochloride ( I-DA), i-L-ascorbic acid (AA) ne-uric acid (UA) ithengwe kwa-Sigma-Aldrich.Wonke ama-reagents asetshenzisiwe ayesezingeni lokuhlaziya futhi asetshenziswa ngaphandle kokuhlanzwa okwengeziwe.
I-NiCo2O4 yahlanganiswa ngendlela elula ye-hydrothermal elandelwa ukwelashwa kokushisa.Kafushane: 1 mmol we-nickel nitrate (Ni(NO3)2∙6H2O) kanye no-2 mmol we-cobalt nitrate (Co(NO3)2∙6H2O) kuhlakazwe ku-30 ​​ml wamanzi acwecwe.Ukuze kulawulwe i-morphology ye-NiCo2O4, izithasiselo ezifana ne-urea, i-ammonium fluoride ne-hexamethylenetetramine (HMT) zengezwe ngokukhetha kulesi sixazululo esingenhla.Yonke ingxube yabe idluliselwa ku-50 ml ye-Teflon-lined autoclave futhi ingaphansi kokusabela kwe-hydrothermal kuhhavini ye-convection ku-120 ° C. amahora angu-6.Ngemva kokupholisa ngokwemvelo kumazinga okushisa asekamelweni, imvula ewumphumela yaba yi-centrifuged futhi igezwe izikhathi eziningana ngamanzi acwengekile ne-ethanol, bese yomiswa ngobusuku obungu-60°C.Ngemva kwalokho, amasampula asanda kulungiswa abalwa ku-400°C amahora angu-4 endaweni ezungezile.Imininingwane yokuhlolwa isohlwini Lwethebula Lolwazi Olwengeziwe S2.
Ukuhlaziywa kwe-X-ray diffraction (XRD, X'Pert-Pro MPD; PANalytical) kwenziwa kusetshenziswa imisebe ye-Cu-Kα (λ = 0.15418 nm) ku-40 kV no-30 mA ukuze kufundwe izakhiwo zesakhiwo zawo wonke ama-nanomaterials e-NCO.Amaphethini okuhluka aqoshwe ebangeni lama-engeli 2θ 10–80° ngesinyathelo esingu-0.05°.I-Surface morphology kanye ne-microstructure yahlolwa kusetshenziswa imakroskopu ye-electron ekhishwayo yasendle (FESEM; Nova SEM 200, FEI) kanye ne-scan transmission electron microscopy (STEM; TALOS F200X, FEI) nge-X-ray spectroscopy (EDS) ehlakaza amandla.Izimo ze-valence ezingaphezulu zahlaziywa nge-X-ray photoelectron spectroscopy (XPS; PHI 5000 Versa Probe II, ULVAC PHI) kusetshenziswa imisebe ye-Al Kα (hν = 1486.6 eV).Amandla okubopha akalwe kusetshenziswa ukuphakama kwe-C 1 ku-284.6 eV njengesithenjwa.Ngemva kokulungisa amasampula ezinhlayiyeni ze-KBR, isibukeli se-Fourier transform infrared (FT-IR) sarekhodwa ebangeni le-wavenumber 1500–400 cm–1 ku-spectrometer ye-Jasco-FTIR-6300.I-Raman spectra iphinde yatholwa kusetshenziswa i-Raman spectrometer (Horiba Co., Japan) ene-He-Ne laser (632.8 nm) njengomthombo wenjabulo.UBrunauer-Emmett-Teller (BET; BELSORP mini II, MicrotracBEL, Corp.) usebenzise i-BELSORP mini II analyzer (MicrotracBEL Corp.) ukukala izinga lokushisa eliphansi le-N2 adsorption-desorption isotherm ukuze balinganisele indawo ethile kanye nokusatshalaliswa kosayizi wembotshana.
Zonke izilinganiso ze-electrochemical, njenge-cyclic voltammetry (CV) ne-chronoamperometry (CA), zenziwe ku-PGSTAT302N potentiostat (Metrohm-Autolab) ekamelweni lokushisa kusetshenziswa isistimu yama-electrode amathathu kusixazululo samanzi esingu-0.1 M NaOH.I-electrode esebenzayo esekelwe ku-glassy carbon electrode (GC), i-electrode ye-Ag/AgCl, nepuleti leplatinamu kwasetshenziswa njenge-electrode esebenzayo, i-electrode eyireferensi, ne-counter electrode, ngokulandelana.Ama-CV aqoshwa phakathi kuka-0 no-0.6 V ngamanani ahlukahlukene wokuskena we-5-100 mV s-1.Ukuze kulinganiswe i-ECSA, i-CV yenziwe ebangeni elingu-0.1-0.2 V ngamanani ahlukahlukene wokuskena (5-100 mV s-1).Thola ukusabela kwe-CA kwesampula ku-glucose ku-0.5 V ngokushukumisa.Ukuze ulinganise ukuzwela nokukhetha, sebenzisa i-glucose engu-0.01–6 mM, 0.1 mM LA, DA, AA, ne-UA ku-0.1 M NaOH.Ukukhiqizwa kabusha kwe-UNCO kwahlolwa kusetshenziswa ama-electrode amathathu ahlukene angezwe ngeglucose engu-5 mM ngaphansi kwezimo ezifanele.Ukuphindaphinda futhi kwahlolwa ngokwenza izilinganiso ezintathu nge-electrode eyodwa ye-UNCO phakathi namahora angu-6.
Yonke idatha ekhiqizwe noma ehlaziywe kulolu cwaningo ifakiwe kulesi sihloko esishicilelwe (kanye nefayela layo lolwazi elingeziwe).
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Isikhathi sokuthumela: Nov-16-2022
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