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Siphande isiphumo sommandla othile womhlaba kwiipropathi ze-electrochemical ze-NiCo2O4 (NCO) zokufumana i-glucose.I-NCO nanomatadium ezinendawo elawulwayo yendawo ethile ziye ziveliswa yi-hydrothermal synthesis kunye ne-additives, kunye ne-self-asembling nanostructures kunye ne-hedgehog, inaliti yepineliti, i-tremella kunye neentyatyambo ezifana ne-morphology nazo zenziwe.Ubutsha bale ndlela ilele kulawulo olucwangcisiweyo lwendlela yokusabela kweekhemikhali ngokongeza izongezo ezahlukeneyo ngexesha lokudibanisa, nto leyo ekhokelela kukwakheka okuzenzekelayo kwee-morphologies ezahlukeneyo ngaphandle kokwahluka kwesakhiwo sekristale kunye nemeko yemichiza yezinto eziyinxalenye.Olu lawulo lwe-morphological lwe-NCO nanomaterials lukhokelela ekutshintsheni okuphawulekayo kwintsebenzo ye-electrochemical yokufumanisa i-glucose.Ngokubambisana nokubonakaliswa kwezinto, ubudlelwane phakathi kwendawo ethile kunye nokusebenza kwe-electrochemical ukufunyanwa kwe-glucose kwaxoxwa.Lo msebenzi unokubonelela ngengqiqo yenzululwazi kwindawo yokulungiswa kwendawo ye-nanostructures emisela ukusebenza kwabo kwizicelo ezinokuthi zibekho kwi-glucose biosensors.
Amanqanaba e-glucose yegazi anika ulwazi olubalulekileyo malunga nemeko ye-metabolic kunye ne-physiological yomzimba1,2.Ngokomzekelo, amanqanaba angaqhelekanga e-glucose emzimbeni angaba ngumqondiso obalulekileyo weengxaki zempilo ezinzulu, kuquka isifo sikashukela, isifo senhliziyo, kunye nokukhuluphala3,4,5.Ngoko ke, ukubeka esweni rhoqo amanqanaba eswekile yegazi kubaluleke kakhulu ekugcineni impilo entle.Nangona iintlobo ezahlukeneyo ze-glucose sensors zisebenzisa ukubonwa kwe-physicochemical ziye zaxelwa, uvakalelo oluphantsi kunye namaxesha okuphendula ngokukhawuleza ahlala engumqobo kwiinkqubo zokubeka iliso ze-glucose eziqhubekayo6,7,8.Ukongezelela, okwangoku i-electrochemical sensors ye-glucose esekelwe kwiimpendulo ze-enzymatic zisenomlinganiselo othile ngaphandle kweenzuzo zabo zokuphendula ngokukhawuleza, uvakalelo oluphezulu kunye neenkqubo ezilula zokwenza izinto9,10.Ngoko ke, iintlobo ezahlukeneyo ze-non-enzymatic electrochemical sensors ziye zafundiswa ngokubanzi ukukhusela i-enzyme denaturation ngelixa zigcina izibonelelo ze-electrochemical biosensors9,11,12,13.
I-Transition metal compounds (TMCs) inomsebenzi ophezulu ngokwaneleyo we-catalytic ngokubhekiselele kwi-glucose, eyandisa ububanzi besicelo sabo kwi-electrochemical glucose sensors13,14,15.Ukuza kuthi ga ngoku, iindlela ezahlukeneyo zoyilo kunye neendlela ezilula zokwenziwa kwe-TMS ziye zacetywa ukuba ziphucule ngakumbi uvakalelo, ukukhetha, kunye nokuzinza kwe-electrochemical yokufumanisa i-glucose16,17,18.Ngokomzekelo, ii-oxide zensimbi eziguquguqukayo ezifana ne-copper oxide (CuO) 11,19, i-zinc oxide (ZnO) 20, i-nickel oxide (NiO) 21,22, i-cobalt oxide (Co3O4) 23,24 kunye ne-cerium oxide (CeO2) i-25 i-electrochemically esebenzayo ngokubhekiselele kwi-glucose.Inkqubela phambili yakutsha nje kwibinary metal oxides ezifana ne-nickel cobaltate (NiCo2O4) yokufunyanwa kweglucose ibonise iziphumo ezongezelelweyo ze-synergistic ngokwemiqathango yokwanda kombane26,27,28,29,30.Ngokukodwa, ukubunjwa okuchanekileyo kunye nokulawulwa kwe-morphology ukwenza i-TMS kunye ne-nanostructures ehlukeneyo inokunyusa ngokufanelekileyo uvakalelo lokubona ngenxa yommandla wabo omkhulu, ngoko ke kucetyiswa kakhulu ukuphuhlisa i-morphology elawulwa yi-TMS yokuphucula ukubonwa kwe-glucose20,25,30,31,32, 33.34, 35.
Apha sibika i-NiCo2O4 (NCO) nanomataterials kunye ne-morphologies eyahlukeneyo yokufunyanwa kwe-glucose.I-NCO nanomaterials ifunyenwe ngendlela elula ye-hydrothermal usebenzisa izongezo ezahlukahlukeneyo, izongezo zekhemikhali zingenye yezinto eziphambili kwi-self-assembly of nanostructures of morphologies eyahlukeneyo.Siphande ngokucwangcisiweyo umphumo we-NCOs ngee-morphologies ezahlukeneyo ekusebenzeni kwabo kwe-electrochemical ukubonwa kwe-glucose, kubandakanywa uvakalelo, ukukhetha, umda ophantsi wokufumanisa, kunye nokuzinza kwexesha elide.
Senze i-NCO nanomaterials (i-UNCO efinyeziweyo, i-PNCO, i-TNCO kunye ne-FNCO ngokulandelanayo) kunye ne-microstructures efana ne-urchins yolwandle, iinaliti zepine, i-tremella kunye neentyatyambo.Umzobo we-1 ubonisa ii-morphologies ezahlukeneyo ze-UNCO, i-PNCO, i-TNCO, kunye ne-FNCO.Imifanekiso ye-SEM kunye nemifanekiso ye-EDS ibonise ukuba i-Ni, i-Co, kunye ne-O yasasazwa ngokulinganayo kwi-NCO nanomaterials, njengoko kuboniswe kwiMifanekiso 1 kunye ne-2. I-S1 kunye ne-S2, ngokulandelanayo.Kwikhiwane.I-2a,b ibonisa ummeli we-TEM imifanekiso ye-NCO nanomaterials ene-morphology eyahlukileyo.I-UNCO yi-self-assembling microsphere (i-diameter: ~ 5 µm) eyenziwe ngee-nanowires ezine-NCO nanoparticles (i-avareji ye-particle size: 20 nm).Le microstructure ekhethekileyo ilindeleke ukuba ibonelele ngommandla omkhulu wokuququzelela ukusasazwa kwe-electrolyte kunye nothutho lwe-electron.Ukongezwa kwe-NH4F kunye ne-urea ngexesha lokudibanisa kubangele i-acicular microstructure (PNCO) 3 µm ubude kunye ne-60 nm ububanzi, eyenziwe ngama-nanoparticles amakhulu.Ukongezwa kwe-HMT endaweni ye-NH4F kubangela i-tremello-like morphology (TNCO) ene-nanosheets ezishwabeneyo.Ukuqaliswa kwe-NH4F kunye ne-HMT ngexesha lokudibanisa kukhokelela ekudityanisweni kwee-nanosheets ezishwabeneyo ezikufutshane, okukhokelela kwi-morphology efana nentyatyambo (FNCO).Umfanekiso we-HREM (umzobo we-2c) ubonisa iibhendi ze-grating ezihlukeneyo ezinezithuba ze-interplanar ze-0.473, 0.278, 0.50, kunye ne-0.237 nm, ehambelana ne-(111), (220), (311), kunye (222) i-NiCo2O4 iindiza, i-27 .Indawo ekhethiweyo ye-electron diffraction pattern (SAED) ye-NCO nanomaterials (inset to Fig. 2b) iphinde yaqinisekisa ubume bepolycrystalline ye-NiCo2O4.Iziphumo ze-high-angle annular imaging emnyama (HAADF) kunye nemephu ye-EDS ibonisa ukuba zonke izinto zihanjiswa ngokulinganayo kwi-NCO nanomaterial, njengoko kuboniswe kwi-Fig 2d.
Umzobo weSchematic wenkqubo yokwenziwa kwe-NiCo2O4 nanostructures ene-morphology elawulwayo.I-Schematics kunye nemifanekiso ye-SEM ye-nanostructures eyahlukeneyo iyaboniswa.
Ukubonakaliswa kwe-morphological kunye nesakhiwo se-NCO nanomaterials: (a) umfanekiso we-TEM, (b) Umfanekiso we-TEM kunye nepateni ye-SAED, (c) umfanekiso we-HRTEM osonjululwe ngokugrumba kunye nemifanekiso ye-HADDF ehambelanayo ye-Ni, Co, kunye ne-O kwi-(d) nanomaterials ye-NCO..
Iipateni ze-X-ray ze-diffraction ye-NCO nanomaterials yee-morphologies ezahlukeneyo ziboniswa kwiFig.3a.I-diffraction iphakamileyo kwi-18.9, 31.1, 36.6, 44.6, 59.1 kunye ne-64.9 ° ibonisa iindiza (111), (220), (311), (400), (511) kunye (440) i-NiCo2O4, ngokulandelanayo, ene-cubic. isakhiwo se-spinel (JCPDS No. 20-0781) 36. I-FT-IR ye-spectra ye-NCO nanomaterials iboniswe kwiiFig.3b.Amaqela amabini anamandla okungcangcazela kummandla phakathi kwe-555 kunye ne-669 cm-1 ihambelana ne-metallic (Ni kunye ne-Co) i-oksijini ethathwe kwi-tetrahedral kunye ne-octahedral positions of the NiCo2O437 spinel, ngokulandelanayo.Ukuqonda ngcono iipropati zesakhiwo se-NCO nanomaterials, i-Raman spectra ifunyenwe njengoko kubonisiwe kwi-Fig. 3c.Iincopho ezine ezibonwe kwi-180, 459, 503, kunye ne-642 cm-1 zihambelana neendlela zeRaman F2g, E2g, F2g, kunye ne-A1g ye-NiCo2O4 spinel, ngokulandelanayo.Imilinganiselo ye-XPS yenziwa ukufumanisa ubume bekhemikhali bomphezulu bezinto kwi-NCO nanomaterials.Kwikhiwane.I-3d ibonisa i-spectrum ye-XPS ye-UNCO.I-spectrum ye-Ni 2p ineencopho ezimbini eziphambili ezibekwe kumandla abophayo we-854.8 kunye ne-872.3 eV, ehambelana ne-Ni 2p3 / 2 kunye ne-Ni 2p1 / 2, kunye neesathelayithi ezimbini ze-vibrational kwi-860.6 kunye ne-879.1 eV, ngokulandelanayo.Oku kubonisa ubukho be-Ni2 + kunye ne-Ni3 + ye-oxidation ithi kwi-NCO.Iincopho ezijikeleze i-855.9 kunye ne-873.4 eV zeze-Ni3+, kunye neencopho ezijikeleze i-854.2 kunye ne-871.6 eV ze-Ni2+.Ngokufanayo, i-spectrum ye-Co2p yee-doubles ze-spin-orbit double ibonisa iincopho ze-Co2 + kunye ne-Co3 + kwi-780.4 (Co 2p3 / 2) kunye ne-795.7 eV (Co 2p1 / 2).I-Peaks kwi-796.0 kunye ne-780.3 eV ihambelana ne-Co2 +, kwaye iphakamileyo kwi-794.4 kunye ne-779.3 eV ihambelana ne-Co3 +.Kufuneka kuqatshelwe ukuba i-polyvalent state ye-ion yensimbi (Ni2 +/ Ni3 + kunye neCo2 +/ Co3 +) kwi-NiCo2O4 ikhuthaza ukwanda komsebenzi we-electrochemical37,38.I-spectra ye-Ni2p kunye ne-Co2p ye-UNCO, i-PNCO, i-TNCO, kunye ne-FNCO ibonise iziphumo ezifanayo, njengoko kuboniswe kumzobo.S3.Ukongezelela, i-spectra ye-O1s yazo zonke i-NCO nanomaterials (i-Fig. S4) ibonise iinqununu ezimbini kwi-592.4 kunye ne-531.2 eV, edibene ne-metal-oxygen kunye neebhondi ze-oksijini kumaqela e-hydroxyl ye-NCO surface, ngokulandelanayo39.Nangona izakhiwo ze-NCO nanomaterials zifana, ukuhlukana kwe-morphological kwii-additives kubonisa ukuba i-additive nganye inokuthatha inxaxheba ngokungafaniyo kwi-chemical reactions ukwenza i-NCO.Oku kulawula i-nucleation ethandeka ngamandla kunye namanyathelo okukhula okuziinkozo, ngaloo ndlela ilawula ubungakanani bamasuntswana kunye neqondo lokudityaniswa kwe-agglomeration.Ke, ukulawulwa kweeparamitha zenkqubo ezahlukeneyo, kubandakanywa izongezo, ixesha lokuphendula, kunye nobushushu ngexesha lokudibanisa, lingasetyenziselwa ukuyila i-microstructure kunye nokuphucula ukusebenza kwe-electrochemical ye-NCO nanomaterials yokufunyanwa kwe-glucose.
(a) Iipatheni ze-X-reyi diffraction, (b) FTIR kunye (c) neRaman spectra yeNCO nanomaterials, (d) i-XPS spectra ye-Ni 2p kunye ne-Co 2p esuka kwi-UNCO.
I-morphology ye-NCO nanomaterials ehlengahlengisiweyo ihambelana ngokusondeleyo nokuqulunqwa kwezigaba zokuqala ezifunyenwe kwiindidi ezahlukahlukeneyo eziboniswe kwi-Figure S5.Ukongeza, i-X-reyi kunye ne-Raman spectra yeesampulu ezisanda kulungiswa (Amanani S6 kunye ne-S7a) abonise ukuba ukubandakanyeka kwezongezo zekhemikhali ezahlukeneyo kubangele ukungafani kwe-crystallographic: i-Ni kunye ne-Co carbonate hydroxides yayibonwa kakhulu kwii-urchins zolwandle kunye nesakhiwo senaliti yompayina, ngelixa njengoko izakhiwo ngendlela ye-tremella kunye neentyatyambo zibonisa ubukho be-nickel kunye ne-cobalt hydroxides.I-FT-IR kunye ne-XPS ye-spectra yeesampuli ezilungisiweyo ziboniswe kwiMifanekiso 1 kunye ne-2. I-S7b-S9 iphinda ibonelele ubungqina obucacileyo bokuhluka okukhankanywe ngasentla kwe-crystallographic.Ukususela kwizinto eziphathekayo zeesampuli ezilungiselelwe, kuyacaca ukuba izongezo zibandakanyeka kwi-hydrothermal reactions kwaye zibonelela ngeendlela ezahlukeneyo zokuphendula ukufumana izigaba zokuqala kunye ne-morphologies eyahlukeneyo40,41,42.I-self-assembly of morphologies eyahlukeneyo, equkethe i-nanowires enye-dimensional (1D) kunye ne-2-dimensional (2D) nanosheets, ichazwa yimeko yeekhemikhali ezahlukeneyo zezigaba zokuqala (i-Ni kunye ne-Co ions, kunye namaqela asebenzayo), ilandelwa yi-crystal growth42, 43, 44, 45, 46, 47. Ngethuba lokulungiswa kwe-post-thermal, izigaba zokuqala ezahlukeneyo ziguqulwa zibe yi-NCO spinel ngelixa zigcina i-morphology yazo ekhethekileyo, njengoko kuboniswe kwiMifanekiso 1 kunye ne-2. 2 kunye ne-3a.
Ukwahlukana kwe-Morphological kwi-NCO nanomaterials kunokuchaphazela indawo ye-electrochemically esebenzayo yokukhangela i-glucose, ngaloo ndlela imisela iimpawu ze-electrochemical jikelele ze-sensor ye-glucose.I-N2 BET adsorption-desorption isotherm yasetyenziselwa ukuqikelela ubungakanani bepore kunye nommandla othile womphezulu weNCO nanomaterials.Kwikhiwane.I-4 ibonisa i-BET isotherms ye-NCO nanomaterials ezahlukeneyo.Ummandla othe ngqo we-BET we-UNCO, i-PNCO, i-TNCO kunye ne-FNCO iqikelelwe kwi-45.303, 43.304, 38.861 kunye ne-27.260 m2 / g, ngokulandelanayo.I-UNCO inommandla ophezulu we-BET womphezulu (45.303 m2 g-1) kunye nomthamo omkhulu wepore (0.2849 cm3 g-1), kunye nokusabalalisa ubungakanani bepore kumxinwa.Iziphumo ze-BET ze-NCO nanomaterials ziboniswe kwiThebhile 1. I-N2 ye-adsorption-desorption curves yayifana kakhulu nohlobo lwe-IV isothermal hysteresis loops, ebonisa ukuba zonke iisampuli zine-mesoporous structure48.Ii-UNCO ze-Mesoporous ezinowona mmandla uphezulu kunye nomthamo ophezulu wepore kulindeleke ukuba zibonelele ngeendawo ezininzi ezisebenzayo zokusabela kwe-redox, ekhokelela kuphuculo lokusebenza kwe-electrochemical.
Iziphumo zeBET ze (a) UNCO, (b) PNCO, (c) TNCO, kunye (d) FNCO.I-inset ibonisa ukuhanjiswa kobungakanani bepore ehambelanayo.
Iimpendulo ze-electrochemical redox ze-NCO nanomataterials ezineemophologies ezahlukeneyo zokufunyanwa kweglucose ziye zavavanywa kusetyenziswa imilinganiselo yeCV.Kwikhiwane.I-5 ibonisa i-CV curves ye-NCO nanomaterials kwi-0.1 M NaOH i-alkaline electrolyte kunye kwaye ngaphandle kwe-5 mM i-glucose kwi-scan rate ye-50 mVs-1.Ukungabikho kwe-glucose, iinqununu ze-redox zabonwa kwi-0.50 kunye ne-0.35 V, ehambelana ne-oxidation ehambelana ne-M-O (M: Ni2 +, Co2 +) kunye ne-M * -O-OH (M *: Ni3 +, Co3 +).usebenzisa iOH anion.Emva kokongezwa kwe-glucose ye-5 mM, ukuphendulwa kwe-redox ebusweni be-NCO nanomaterials kwanda kakhulu, okunokuthi kube ngenxa ye-oxidation ye-glucose kwi-gluconolactone.Umzobo we-S10 ubonisa i-peak redox currents kumazinga okuskena kwe-5-100 mV s-1 kwisisombululo se-0.1 M NaOH.Kucacile ukuba i-peak redox yangoku iyanda ngokunyuka kwezinga lokuskena, ebonisa ukuba i-NCO nanomaterials ine-diffusion efanayo elawulwa ukuziphatha kwe-electrochemical50,51.Njengoko kuboniswe kwi-Figure S11, indawo ye-electrochemical surface (ECSA) ye-UNCO, i-PNCO, i-TNCO, kunye ne-FNCO iqikelelwa ukuba yi-2.15, 1.47, 1.2, kunye ne-1.03 cm2, ngokulandelanayo.Oku kuphakamisa ukuba i-UNCO iluncedo kwinkqubo ye-electrocatalytic, iququzelele ukufunyanwa kwe-glucose.
Iigophe ze-CV (a) i-UNCO, (b) i-PNCO, (c) i-TNCO, kunye (d) nee-electrodes ze-FNCO ezingenayo i-glucose kwaye zongezwa nge-5 mM glucose ngesantya sokuskena se-50 mVs-1.
Ukusebenza kwe-electrochemical ye-NCO nanomaterials yokukhangela i-glucose yaphandwa kwaye iziphumo ziboniswe kwi-Fig. 6. Ukukhathazeka kwe-glucose kunqunywe yindlela ye-CA ngokongezwa kwe-stepwise ye-concentrations eyahlukeneyo ye-glucose (0.01-6 mM) kwi-0.1 M isisombululo se-NaOH kwi-0.5 V kunye nekhefu le-60 s.Njengoko kubonisiwe kwifig.I-6a-d, i-NCO nanomaterials ibonisa uvakalelo oluhlukeneyo ukusuka kwi-84.72 ukuya kwi-116.33 µA mM-1 cm-2 ene-coefficients ephezulu yokulungelelanisa (R2) ukusuka kwi-0.99 ukuya kwi-0.993.Ijika lokulinganisa phakathi koxinzelelo lwe-glucose kunye nokuphendula kwangoku kwe-NCO nanomaterials kuboniswe kumkhiwane.S12.Imida ebaliweyo yokufunyanwa (LOD) ye-NCO nanomaterials yayikuluhlu lwe-0.0623-0.0783 µM.Ngokweziphumo zovavanyo lwe-CA, i-UNCO ibonise uvakalelo oluphezulu (116.33 μA mM-1 cm-2) kuluhlu olubanzi lokufumanisa.Oku kunokucaciswa ngemo engafaniyo neyolwandle efana neurchin yolwandle, equlathe isakhelo se-mesoporous esinendawo enkulu yomphezulu ebonelela ngeendawo ezininzi ezisebenzayo zeentlobo zeglucose.Ukusebenza kwe-electrochemical ye-NCO nanomaterials evezwe kwiThebhile S1 iqinisekisa ukusebenza okugqwesileyo kwe-electrochemical glucose ye-NCO nanomaterials elungiselelwe kolu phononongo.
Iimpendulo ze-CA ze-UNCO (a), i-PNCO (b), i-TNCO (c), kunye ne-FNCO (d) i-electrodes ene-glucose eyongeziweyo kwi-0.1 M isisombululo se-NaOH kwi-0.50 V. I-insets ibonisa i-curves yokulinganisa iimpendulo zangoku ze-NCO nanomaterials: (e ) Iimpendulo ze-KA ze-UNCO, (f) i-PNCO, (g) i-TNCO, kunye (h) ne-FNCO ngokongezwa kwe-1 mM ye-glucose kunye ne-0.1 mM izinto eziphazamisayo (LA, DA, AA, kunye ne-UA).
Ikhono lokuchasana nokuphazamiseka kokufunyanwa kwe-glucose enye into ebalulekileyo ekubonweni okukhethiweyo kunye nokukhathazeka kwe-glucose ngokuphazamisa iikhompawundi.Kwikhiwane.I-6e-h ibonisa amandla okuthintela ukuphazamiseka kwe-NCO nanomaterials kwi-0.1 M isisombululo se-NaOH.Iimolekyuli eziqhelekileyo eziphazamisayo ezifana ne-LA, DA, AA kunye ne-UA zikhethiweyo kwaye zongezwa kwi-electrolyte.Impendulo yangoku ye-NCO nanomaterials kwi-glucose ibonakala.Nangona kunjalo, impendulo yangoku kwi-UA, DA, AA kunye ne-LA ayizange itshintshe, oku kuthetha ukuba i-NCO nanomaterials ibonise ukhetho oluhle kakhulu lokukhangela i-glucose kungakhathaliseki ukuhlukana kwabo kwe-morphological.Umzobo we-S13 ubonisa ukuzinza kwe-NCO nanomaterials ehlolwe yi-CA impendulo kwi-0.1 M NaOH, apho i-glucose ye-1 mM yongezwa kwi-electrolyte ixesha elide (80,000 s).Iimpendulo zangoku ze-UNCO, i-PNCO, i-TNCO, kunye ne-FNCO ziyi-98.6%, i-97.5%, i-98.4%, kunye ne-96.8%, ngokulandelanayo, yeyokuqala ngoku kunye nokongezwa kwe-glucose ye-1 mM eyongezelelweyo emva kwe-80,000 s.Zonke i-NCO nanomaterials zibonisa ukuphendulwa kwe-redox ezinzile kunye neentlobo ze-glucose kwixesha elide.Ngokukodwa, isibonakaliso sangoku se-UNCO asigcinanga kuphela i-97.1% ye-97.1% ye-current yokuqala, kodwa iphinde igcine i-morphology kunye neempawu zebhondi yeekhemikhali emva kovavanyo lokuzinza kokusingqongileyo lweentsuku ezi-7 (Amanani S14 kunye ne-S15a).Ukongezelela, ukuveliswa kunye nokuveliswa kwe-UNCO kwavavanywa njengoko kuboniswe kwi-Fig. S15b, c.I-Relative Standard Deviation (i-RSD) ebaliweyo yokuphindaphinda kunye nokuphindaphinda yayiyi-2.42% kunye ne-2.14%, ngokulandelanayo, ebonisa izicelo ezinokubakho njenge-industrial grade grade sensor.Oku kubonisa ukuzinza okugqwesileyo kolwakhiwo kunye neekhemikhali ze-UNCO phantsi kweemeko ze-oxidizing zokubona i-glucose.
Kucacile ukuba ukusebenza kwe-electrochemical ye-NCO nanomaterials yokukhangela i-glucose ihambelana kakhulu neenzuzo zesakhiwo sesigaba sokuqala esilungiselelwe yindlela ye-hydrothermal kunye ne-additives (Fig. S16).Ummandla ophezulu we-UNCO uneendawo ezininzi ze-electroactive kunezinye i-nanostructures, ezinceda ukuphucula ukusabela kwe-redox phakathi kwezinto ezisebenzayo kunye neengqungquthela ze-glucose.Isakhiwo se-mesoporous se-UNCO sinokutyhila ngokulula ngakumbi iisayithi ze-Ni kunye ne-Co kwi-electrolyte ukubhaqa i-glucose, okukhokelela ekuphenduleni ngokukhawuleza kwe-electrochemical.I-nanowires ene-dimensional enye kwi-UNCO inokunyusa ngakumbi isantya sokusasazwa ngokubonelela ngeendlela ezimfutshane zothutho zee-ion kunye nee-electron.Ngenxa yeempawu ezikhethekileyo zesakhiwo ezikhankanywe ngasentla, ukusebenza kwe-electrochemical ye-UNCO yokubona i-glucose iphezulu kune-PNCO, i-TNCO, kunye ne-FNCO.Oku kubonisa ukuba i-morphology ye-UNCO ekhethekileyo kunye neyona ndawo iphakamileyo kunye nobukhulu be-pore inokubonelela ngokusebenza okugqwesileyo kwe-electrochemical ukubonwa kwe-glucose.
Umphumo wendawo ethile yendawo kwiimpawu ze-electrochemical ze-NCO nanomaterials zafundwa.I-NCO nanomaterials kunye nommandla ohlukeneyo wendawo ethile ifunyenwe ngendlela elula ye-hydrothermal kunye nezongezo ezahlukeneyo.Izongezo ezahlukeneyo ngexesha lokudibanisa zingena kwiimpendulo zeekhemikhali ezahlukeneyo kwaye zenze izigaba zokuqala ezahlukeneyo.Oku kuye kwakhokelela ekuzihlanganiseni kwe-nanostructures eyahlukeneyo kunye ne-morphology efana ne-hedgehog, inaliti yepine, i-tremella, kunye nentyatyambo.I-post-heating elandelayo ikhokelela kwimeko efanayo yeekhemikhali ze-crystalline ze-NCO nanomaterials kunye nesakhiwo se-spinel ngelixa ligcina i-morphology yazo ekhethekileyo.Ngokuxhomekeke kwindawo engaphezulu ye-morphology eyahlukileyo, ukusebenza kwe-electrochemical ye-NCO nanomaterials yokufunyanwa kweglucose kuphuculwe kakhulu.Ngokukodwa, i-glucose sensitivity ye-NCO nanomaterials ene-urchin morphology yolwandle yanda ukuya kwi-116.33 µA mM-1 cm-2 kunye ne-coefficient ephezulu yokulungelelanisa (R2) ye-0.99 kwi-linear range ye-0.01-6 mM.Lo msebenzi unokubonelela ngesiseko senzululwazi sobunjineli be-morphological ukulungelelanisa indawo ethile yomhlaba kunye nokuphucula ngakumbi ukusebenza kwe-electrochemical ye-non-enzymatic biosensor applications.
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) kunye ne-uric acid (UA) yathengwa kwi-Sigma-Aldrich.Zonke ii-reagents ezisetyenzisiweyo bezikwibakala lokuhlalutya kwaye zasetyenziswa ngaphandle kokucocwa ngakumbi.
I-NiCo2O4 yenziwe ngendlela elula ye-hydrothermal elandelwa kunyango lobushushu.Ngokufutshane: i-1 mmol ye-nickel nitrate (Ni(NO3) 2∙6H2O) kunye ne-2 mmol ye-cobalt nitrate (Co (NO3) 2∙6H2O) yachithwa kwi-30 ml yamanzi adibeneyo.Ukuze ulawule i-morphology ye-NiCo2O4, izongezo ezifana ne-urea, i-ammonium fluoride kunye ne-hexamethylenetetramine (HMT) zongezwa ngokukhethiweyo kwisisombululo esingentla.Umxube wonke emva koko udluliselwe kwi-50 ml ye-Teflon-lined autoclave kwaye ixhomekeke kwi-hydrothermal reaction kwi-oven convection kwi-120 ° C. iiyure ze-6.Emva kokupholisa kwendalo kwiqondo lobushushu begumbi, i-precipitate ebangele i-centrifuged kwaye ihlanjwe amaxesha amaninzi ngamanzi adibeneyo kunye ne-ethanol, kwaye yomiswa ngobusuku kwi-60 ° C.Emva koko, iisampuli ezisandul 'ukulungiswa zifakwe kwi-400 ° C kwi-4 h kwi-atmosphere ye-ambient.Iinkcukacha zovavanyo zidweliswe kwiTheyibhile yoLwazi oloNgezelelweyo S2.
Uhlalutyo lwe-X-ray diffraction (i-XRD, i-X'Pert-Pro MPD; i-PANalytical) yenziwe ngokusebenzisa i-Cu-Kα radiation (λ = 0.15418 nm) kwi-40 kV kunye ne-30 mA ukufunda iimpawu zesakhiwo kuzo zonke i-NCO nanomaterials.Iipateni ze-diffraction zirekhodwe kuluhlu lwee-angles 2θ 10-80 ° kunye nesinyathelo se-0.05 °.I-Scan morphology kunye ne-microstructure yavavanywa kusetyenziswa i-emission emission electron microscopy (FESEM; Nova SEM 200, FEI) kunye ne-electron microscopy yokuhanjiswa kwe-scan (STEM; TALOS F200X, FEI) kunye ne-X-ray spectroscopy (EDS).I-valence state of the surface yahlalutywa nge-X-ray photoelectron spectroscopy (XPS; PHI 5000 Versa Probe II, ULVAC PHI) usebenzisa i-Al Kα radiation (hν = 1486.6 eV).Amandla okubopha alinganiswe kusetyenziswa i-C 1 s peak kwi-284.6 eV njengesalathisi.Emva kokulungiselela iisampulu kwiisuntswana ze-KBR, i-Fourier transform infrared (FT-IR) spectra ibhalwe kwi-wavenumber range 1500-400 cm-1 kwi-spectrometer ye-Jasco-FTIR-6300.I-Raman spectra nayo yafunyanwa kusetyenziswa i-Raman spectrometer (Horiba Co., Japan) ene-laser ye-He-Ne (632.8 nm) njengomthombo wochulumanco.I-Brunauer-Emmett-Teller (BET; BELSORP mini II, MicrotracBEL, Corp.) isebenzise i-BELSORP mini II analyzer (MicrotracBEL Corp.) ukulinganisa iqondo lokushisa eliphantsi le-N2 i-adsorption-desorption isotherms ukuqikelela indawo ethile yendawo kunye nokusabalalisa ubukhulu bepore.
Zonke izilinganiso ze-electrochemical, ezifana ne-cyclic voltammetry (CV) kunye ne-chronoamperometry (CA), zenziwa kwi-PGSTAT302N potentiostat (i-Metrohm-Autolab) kwiqondo lokushisa lokushisa usebenzisa inkqubo ye-electrode emithathu kwi-0.1 M i-NaOH isisombululo samanzi.I-electrode esebenzayo esekelwe kwi-glassy carbon electrode (GC), i-electrode ye-Ag / AgCl, kunye neplatinum plate isetyenziswe njenge-electrode esebenzayo, i-electrode yereferensi, kunye ne-counter electrode, ngokulandelanayo.Ii-CVs zarekhodwa phakathi kwe-0 kunye ne-0.6 V kwiireyithi ezahlukeneyo zokuskena ze-5-100 mV s-1.Ukulinganisa i-ECSA, i-CV yenziwa kuluhlu lwe-0.1-0.2 V kumazinga ahlukeneyo okuskena (5-100 mV s-1).Fumana isampula ye-CA reaction yeglucose kwi-0.5 V ngokuvuselela.Ukulinganisa uvakalelo kunye nokukhetha, sebenzisa i-0.01-6 mM glucose, 0.1 mM LA, DA, AA, kunye ne-UA kwi-0.1 M NaOH.Ukuveliswa kwakhona kwe-UNCO kwavavanywa kusetyenziswa i-electrode ezintathu ezahlukeneyo zongezwa nge-5 mM glucose phantsi kweemeko ezifanelekileyo.Ukuphindaphinda kwakhona kwajongwa ngokwenza imilinganiselo emithathu nge-electrode ye-UNCO enye kwiiyure ze-6.
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