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Tidafufuza momwe malo enaake amagwirira ntchito pamagetsi a electrochemical a NiCo2O4 (NCO) kuti azindikire shuga.NCO nanomatadium zokhala ndi malo olamulidwa enieni apangidwa ndi hydrothermal synthesis yokhala ndi zowonjezera, komanso zodziphatikiza zokha ndi hedgehog, singano ya paini, tremella ndi maluwa ngati morphology apangidwanso.The zachilendo njira yagona mu kulamulira mwadongosolo njira mankhwala anachita powonjezera zina zosiyanasiyana pa kaphatikizidwe, zomwe zimabweretsa mowiriza mapangidwe morphologies zosiyanasiyana popanda kusiyana kristalo dongosolo ndi boma mankhwala a zinthu constituent.Kuwongolera kwa morphological kwa NCO nanomatadium kumabweretsa kusintha kwakukulu pakuchita kwa electrochemical pakuzindikira shuga.Molumikizana ndi mawonekedwe azinthu, ubale pakati pa malo enieni ndi magwiridwe antchito a electrochemical pakuzindikira glucose adakambidwa.Ntchitoyi ikhoza kupereka chidziwitso chasayansi pakusintha kwapamwamba kwa ma nanostructures omwe amatsimikizira momwe angagwiritsire ntchito pakugwiritsa ntchito ma glucose biosensors.
Miyezo ya shuga m'magazi imapereka chidziwitso chofunikira chokhudza kagayidwe kachakudya ndi momwe thupi limakhalira1,2.Mwachitsanzo, kuchuluka kwa shuga m'thupi mwachilendo kumatha kukhala chizindikiro chofunikira chamavuto akulu azaumoyo, kuphatikiza matenda a shuga, matenda amtima, ndi kunenepa kwambiri3,4,5.Chifukwa chake, kuyang'anira kuchuluka kwa shuga m'magazi ndikofunikira kwambiri kuti mukhale ndi thanzi labwino.Ngakhale mitundu yosiyanasiyana ya masensa a shuga pogwiritsa ntchito kuzindikira kwa physicochemical yanenedwa, kukhudzika kochepa komanso nthawi yoyankha pang'onopang'ono kumakhalabe zolepheretsa kupitiliza kuyang'anira shuga6,7,8.Kuphatikiza apo, masensa odziwika a glucose a electrochemical pakali pano otengera ma enzymatic reaction akadali ndi zofooka zina ngakhale zabwino zake zakuyankha mwachangu, kukhudzika kwakukulu komanso njira zosavuta zopangira9,10.Choncho, mitundu yosiyanasiyana ya ma electrochemical sensors omwe sali a enzymatic yakhala ikuphunziridwa mozama kuti ateteze enzyme denaturation pamene akusunga ubwino wa electrochemical biosensors9,11,12,13.
Transition metal compounds (TMCs) zimakhala ndi mphamvu zokwanira zogwiritsira ntchito shuga, zomwe zimakulitsa kuchuluka kwa momwe zimagwiritsidwira ntchito pamagetsi a electrochemical glucose sensors13,14,15.Pakalipano, mapangidwe osiyanasiyana omveka bwino ndi njira zosavuta zopangira TMS zaperekedwa kuti zipititse patsogolo kukhudzidwa, kusankha, ndi kukhazikika kwa electrochemical kuzindikirika kwa glucose16,17,18.Mwachitsanzo, mosadziwika bwino kusintha zitsulo oxides monga mkuwa okusayidi (CuO) 11,19, nthaka okusayidi (ZnO) 20, nickel okusayidi (NiO) 21,22, cobalt okusayidi (Co3O4) 23,24 ndi cerium okusayidi (CeO2) 25 ndi electrochemically yogwira pokhudzana ndi glucose.Kupita patsogolo kwaposachedwa kwa ma oxides achitsulo monga nickel cobaltate (NiCo2O4) pozindikira shuga kwawonetsa zina zowonjezera zokhudzana ndi kuchuluka kwamagetsi26,27,28,29,30.Makamaka, kuwongolera kolondola komanso kuwongolera ma morphology kuti apange TMS yokhala ndi ma nanostructures osiyanasiyana amatha kukulitsa chidwi chodziwikiratu chifukwa cha malo awo akuluakulu, chifukwa chake tikulimbikitsidwa kupanga TMS yoyendetsedwa ndi morphology kuti idziwe bwino shuga20,25,30,31,32, 33.34, 35.
Apa tikuwonetsa ma Nanomatadium a NiCo2O4 (NCO) okhala ndi ma morphologies osiyanasiyana ozindikira shuga.NCO nanomatadium amapezedwa ndi njira yosavuta ya hydrothermal pogwiritsa ntchito zowonjezera zosiyanasiyana, zowonjezera za mankhwala ndi chimodzi mwazinthu zofunika pakudzipangira nokha ma nanostructures osiyanasiyana a morphologies.Tidafufuza mwadongosolo momwe ma NCO amagwirira ntchito ndi ma morphologies osiyanasiyana pakuchita kwawo kwa electrochemical kuti azindikire shuga, kuphatikiza kukhudzika, kusankha, kuchepetsa kuzindikira, komanso kukhazikika kwanthawi yayitali.
Tidapanga NCO nanomatadium (chidule cha UNCO, PNCO, TNCO ndi FNCO motsatana) chokhala ndi tinthu tating'onoting'ono tofanana ndi ma urchins am'nyanja, singano zapaini, tremella ndi maluwa.Chithunzi 1 chikuwonetsa ma morphology osiyanasiyana a UNCO, PNCO, TNCO, ndi FNCO.Zithunzi za SEM ndi zithunzi za EDS zimasonyeza kuti Ni, Co, ndi O adagawidwa mofanana mu nanomaterials ya NCO, monga momwe tawonetsera mu Zithunzi 1 ndi 2. S1 ndi S2, motsatira.Pa mkuyu.2a,b ikuwonetsa zithunzi za TEM zoyimira za NCO nanomatadium zokhala ndi morphology yosiyana.UNCO ndi microsphere yodzipangira yokha (m'mimba mwake: ~ 5 µm) yopangidwa ndi nanowires ndi NCO nanoparticles (avareji ya tinthu tating'ono: 20 nm).Microstructure yapaderayi ikuyembekezeka kupatsa malo akulu kuti athandizire kufalikira kwa ma electrolyte ndi mayendedwe amagetsi.Kuphatikizika kwa NH4F ndi urea panthawi ya kaphatikizidwe kunapangitsa kuti acicular acicular microstructure (PNCO) 3 µm kutalika ndi 60 nm m'lifupi, yopangidwa ndi nanoparticles zazikulu.Kuwonjezeredwa kwa HMT m'malo mwa NH4F kumabweretsa morphology yofanana ndi tremello (TNCO) yokhala ndi ma nanosheets okwinya.Kuyambitsidwa kwa NH4F ndi HMT panthawi yophatikizika kumabweretsa kuphatikizika kwa ma nanosheets oyandikana nawo, zomwe zimapangitsa kuti pakhale mawonekedwe ngati maluwa (FNCO).Chithunzi cha HREM (mkuyu 2c) chikuwonetsa magulu opangira ma grating omwe ali ndi ma interplanar spacings a 0.473, 0.278, 0.50, ndi 0.237 nm, ofanana ndi (111), (220), (311), ndi (222) NiCo2O4 ndege, s 27 .Anasankha m'dera elekitironi diffraction chitsanzo (SAED) wa NCO nanomaterials (kuyika kwa mkuyu. 2b) anatsimikiziranso polycrystalline chikhalidwe cha NiCo2O4.Zotsatira za high-angle annular imaging dark (HAADF) ndi mapu a EDS amasonyeza kuti zinthu zonse zimagawidwa mofanana mu NCO nanomaterial, monga momwe tawonetsera mkuyu 2d.
Chithunzi chadongosolo la mapangidwe a NiCo2O4 nanostructures okhala ndi morphology yoyendetsedwa.Zithunzi za Schematics ndi SEM zama nanostructures osiyanasiyana zimawonetsedwanso.
morphological and structural characterization of NCO nanomaterials: (a) TEM image, (b) TEM image pamodzi ndi SAED pattern, (c) grating-resolved HRTEM image and molingana HADDF images of Ni, Co, and O in (d) NCO nanomaterials..
Ma X-ray diffraction machitidwe a NCO nanomaterials a morphologies osiyanasiyana akuwonetsedwa mu Mkuyu.3 a.The diffraction nsonga pa 18.9, 31.1, 36.6, 44.6, 59.1 ndi 64.9 ° amasonyeza ndege (111), (220), (311), (400), (511) ndi (440) NiCo2O4, motero, amene ali kiyubiki kapangidwe ka spinel (JCPDS No. 20-0781) 36. Mawonekedwe a FT-IR a NCO nanomaterials akuwonetsedwa mu Mkuyu.3b .Magulu awiri amphamvu ogwedezeka m'derali pakati pa 555 ndi 669 cm-1 amafanana ndi zitsulo (Ni ndi Co) mpweya wochokera ku tetrahedral ndi octahedral positions of NiCo2O437 spinel, motsatira.Kuti mumvetse bwino mapangidwe a NCO nanomaterials, zojambula za Raman zinapezedwa monga momwe tawonetsera mkuyu 3c.Mapiri anayi omwe amawonedwa pa 180, 459, 503, ndi 642 cm-1 amagwirizana ndi mitundu ya Raman F2g, E2g, F2g, ndi A1g ya NiCo2O4 spinel, motsatana.Miyezo ya XPS idachitidwa kuti adziwe momwe zinthu zilili mu NCO nanomatadium.Pa mkuyu.3d ikuwonetsa mawonekedwe a XPS a UNCO.Sipekitiramu ya Ni 2p ili ndi nsonga zazikulu ziwiri zomwe zili pamphamvu zomangirira za 854.8 ndi 872.3 eV, zofananira ndi Ni 2p3/2 ndi Ni 2p1/2, ndi ma satellites awiri onjenjemera pa 860.6 ndi 879.1 eV, motsatana.Izi zikuwonetsa kukhalapo kwa mayiko a Ni2+ ndi Ni3+ oxidation ku NCO.Nsonga zozungulira 855.9 ndi 873.4 eV ndi za Ni3+, ndipo nsonga zozungulira 854.2 ndi 871.6 eV ndi za Ni2+.Momwemonso, mawonekedwe a Co2p a ma spin-orbit doublet amawulula nsonga zapamwamba za Co2+ ndi Co3+ pa 780.4 (Co 2p3/2) ndi 795.7 eV (Co 2p1/2).Pamwamba pa 796.0 ndi 780.3 eV amafanana ndi Co2+, ndipo nsonga za 794.4 ndi 779.3 eV zimagwirizana ndi Co3+.Kuyenera kudziŵika kuti polyvalent boma la ayoni zitsulo (Ni2 +/ Ni3 + ndi Co2 +/ Co3 +) mu NiCo2O4 amalimbikitsa kuwonjezeka electrochemical ntchito37,38.Mawonekedwe a Ni2p ndi Co2p a UNCO, PNCO, TNCO, ndi FNCO adawonetsa zotsatira zofanana, monga zikuwonetsedwa mkuyu.S3.Komanso, mawonekedwe a O1s a NCO nanomaterials onse (mkuyu. S4) adawonetsa nsonga ziwiri pa 592.4 ndi 531.2 eV, zomwe zimagwirizanitsidwa ndi zomangira zachitsulo-oxygen ndi mpweya m'magulu a hydroxyl a NCO pamwamba, motero39.Ngakhale kuti mapangidwe a NCO nanomatadium ali ofanana, kusiyana kwa morphological kwa zowonjezera kumasonyeza kuti chowonjezera chilichonse chikhoza kutenga nawo mbali mosiyanasiyana pakupanga mankhwala kuti apange NCO.Izi amazilamulira mwamphamvu yabwino nucleation ndi mbewu kukula masitepe, potero kulamulira tinthu kukula ndi digiri ya agglomeration.Chifukwa chake, kuwongolera magawo osiyanasiyana azinthu, kuphatikiza zowonjezera, nthawi yochitira, ndi kutentha panthawi ya kaphatikizidwe, zitha kugwiritsidwa ntchito kupanga ma microstructure ndikuwongolera magwiridwe antchito a electrochemical a NCO nanomaterials kuti azindikire shuga.
(a) Maonekedwe a X-ray, (b) FTIR ndi (c) Raman spectra of NCO nanomaterials, (d) XPS spectra of Ni 2p and Co 2p from UNCO.
Mapangidwe a ma NCO nanomatadium omwe adasinthidwa amagwirizana kwambiri ndi mapangidwe a magawo oyambira omwe amapezeka kuchokera pazowonjezera zosiyanasiyana zomwe zikuwonetsedwa mu Chithunzi S5.Komanso, X-ray ndi Raman sipekitiramu wa zitsanzo mwatsopano okonzeka (Figures S6 ndi S7a) anasonyeza kuti nawo osiyana mankhwala zina zinachititsa crystallographic kusiyana: Ni ndi Co carbonate hydroxides makamaka ankaona urchins nyanja ndi paini singano dongosolo, pamene monga mapangidwe amtundu wa tremella ndi maluwa akuwonetsa kukhalapo kwa nickel ndi cobalt hydroxides.Mawonekedwe a FT-IR ndi XPS a zitsanzo zokonzekera akuwonetsedwa mu Zithunzi 1 ndi 2. S7b-S9 imaperekanso umboni womveka bwino wa kusiyana kwa crystallographic komwe tatchula.Kuchokera kuzinthu zakuthupi zomwe zakonzedwa, zikuwonekeratu kuti zowonjezera zimakhudzidwa ndi machitidwe a hydrothermal ndikupereka njira zosiyana zopezera magawo oyambirira ndi morphologies osiyana40,41,42.Kudziphatika kwa ma morphologies osiyanasiyana, opangidwa ndi mbali imodzi (1D) nanowires ndi ma nanosheets awiri-dimensional (2D), akufotokozedwa ndi mitundu yosiyanasiyana ya mankhwala a magawo oyambirira (Ni ndi Co ions, komanso magulu ogwira ntchito), kutsatiridwa ndi kukula kwa kristalo42, 43, 44, 45, 46, 47. Pakafukufuku wotentha kwambiri, magawo osiyanasiyana oyambirira amasandulika kukhala NCO spinel pamene akusunga morphology yawo yapadera, monga momwe tawonetsera mu Zithunzi 1 ndi 2. 2 ndi 3a.
Kusiyana kwa morphological mu NCO nanomatadium kumatha kukhudza gawo la electrochemically yogwira ntchito kuti lizindikire shuga, potero kudziwa mawonekedwe a electrochemical a sensa ya glucose.N2 BET adsorption-desorption isotherm idagwiritsidwa ntchito kuyerekeza kukula kwa pore ndi malo enaake a NCO nanomatadium.Pa mkuyu.4 ikuwonetsa ma isotherms a BET amitundu yosiyanasiyana ya NCO nanomatadium.Malo enieni a BET a UNCO, PNCO, TNCO ndi FNCO adayesedwa pa 45.303, 43.304, 38.861 ndi 27.260 m2 / g, motero.UNCO ili ndi malo apamwamba kwambiri a BET (45.303 m2 g-1) komanso voliyumu yayikulu kwambiri ya pore (0.2849 cm3 g-1), ndipo kukula kwa pore ndikocheperako.Zotsatira za BET za NCO nanomaterials zikuwonetsedwa mu Table 1. Mapiritsi a N2 adsorption-desorption anali ofanana kwambiri ndi mtundu wa IV isothermal hysteresis loops, kusonyeza kuti zitsanzo zonse zinali ndi mesoporous structure48.Ma UNCO a Mesoporous omwe ali ndi malo okwera kwambiri komanso kuchuluka kwa pore akuyembekezeredwa kuti apereke malo ambiri ochitirapo ma redox, zomwe zimapangitsa kuti ma electrochemical agwire bwino ntchito.
Zotsatira za BET za (a) UNCO, (b) PNCO, (c) TNCO, ndi (d) FNCO.Tsambali likuwonetsa kukula kwa pore kofananira.
Ma electrochemical redox reaction of NCO nanomatadium okhala ndi ma morphologies osiyanasiyana ozindikira shuga adawunikidwa pogwiritsa ntchito miyeso ya CV.Pa mkuyu.5 ikuwonetsa ma curve a CV a NCO nanomaterials mu 0.1 M NaOH alkaline electrolyte yokhala ndi shuga wa 5 mm komanso wopanda 5 mM pa sikani ya 50 mVs-1.Popanda shuga, nsonga za redox zidawonedwa pa 0.50 ndi 0.35 V, zofananira ndi okosijeni wolumikizidwa ndi M-O (M: Ni2+, Co2+) ndi M *-O-OH (M*: Ni3+, Co3+).pogwiritsa ntchito OH anion.Pambuyo Kuwonjezera 5 mm shuga, ndi redox anachita padziko la nanomaterials NCO kwambiri kuchuluka, amene mwina chifukwa makutidwe ndi okosijeni wa shuga kuti gluconolactone.Chithunzi S10 chikuwonetsa kuchuluka kwa mafunde a redox pamasinthidwe a 5-100 mV s-1 mu yankho la 0.1 M NaOH.Zikuwonekeratu kuti nsonga ya redox panopa ikuwonjezeka ndi kuchuluka kwa scan scan, kusonyeza kuti NCO nanomaterials ali ndi kufalikira kofanana komwe kumayendetsedwa ndi electrochemical behaviour50,51.Monga momwe tawonetsera mu Chithunzi S11, malo a electrochemical surface (ECSA) a UNCO, PNCO, TNCO, ndi FNCO akuyerekezedwa kukhala 2.15, 1.47, 1.2, ndi 1.03 cm2, motsatira.Izi zikuwonetsa kuti UNCO ndiyothandiza pamachitidwe a electrocatalytic, kuthandizira kuzindikira kwa glucose.
Ma CV ma curve a (a) UNCO, (b) PNCO, (c) TNCO, ndi (d) maelekitirodi a FNCO opanda shuga komanso ophatikizidwa ndi 5 mM glucose pamlingo wa 50 mVs-1.
Ma electrochemical performance a NCO nanomatadium pozindikira shuga adafufuzidwa ndipo zotsatira zake zikuwonetsedwa mu chithunzi 6. Kukhudzika kwa shuga kunatsimikiziridwa ndi njira ya CA powonjezera pang'onopang'ono kuchuluka kwa shuga (0.01-6 mM) mu 0.1 M NaOH yankho pa 0.5 V ndi nthawi ya 60s.Monga momwe tawonetsera mkuyu.6a–d, NCO nanomatadium amawonetsa kukhudzika kosiyana kuyambira 84.72 mpaka 116.33 µA mM-1 cm-2 yokhala ndi ma coefficients apamwamba (R2) kuchokera ku 0.99 mpaka 0.993.Kupindika kwa ma calibration pakati pa kuchuluka kwa shuga ndi momwe ma NCO nanomatadium amachitira akuwonetsedwa mkuyu.S12.Malire owerengeredwa ozindikira (LOD) a NCO nanomatadium anali mumitundu ya 0.0623–0.0783 µM.Malinga ndi zotsatira za mayeso a CA, UNCO inasonyeza kukhudzidwa kwambiri (116.33 μA mM-1 cm-2) pamtundu wambiri wodziwika.Izi zitha kufotokozedwa ndi mawonekedwe ake apadera amtundu wa urchin wa m'nyanja, wokhala ndi mawonekedwe a mesoporous okhala ndi malo akuluakulu apadera omwe amapereka malo ambiri opangira mitundu ya shuga.Kachitidwe ka electrochemical ka NCO nanomatadium zomwe zaperekedwa mu Table S1 zimatsimikizira magwiridwe antchito a electrochemical glucose wa NCO nanomatadium zokonzedwa mu kafukufukuyu.
Mayankho a CA a UNCO (a), PNCO (b), TNCO (c), ndi maelekitirodi a FNCO (d) okhala ndi shuga wowonjezedwa ku njira ya 0.1 M NaOH pa 0.50 V. Zolembazi zikuwonetsa ma curve osinthika a mayankho apano a NCO nanomaterials: (e ) Mayankho a KA a UNCO, (f) PNCO, (g) TNCO, ndi (h) FNCO powonjezera pang'onopang'ono 1 mM glucose ndi 0.1 mM interfering substances (LA, DA, AA, ndi UA).
Kuthekera kolimbana ndi kusokoneza kwa kuzindikira kwa glucose ndi chinthu china chofunikira pakusankha komanso kuzindikira kwamphamvu kwa glucose posokoneza zinthu.Pa mkuyu.6e–h ikuwonetsa kuthekera kothana ndi kusokoneza kwa NCO nanomatadium mu 0.1 M NaOH yankho.Mamolekyu osokoneza wamba monga LA, DA, AA ndi UA amasankhidwa ndikuwonjezeredwa ku electrolyte.Mayankho apano a NCO nanomatadium ku glucose akuwonekera.Komabe, kuyankha kwaposachedwa kwa UA, DA, AA ndi LA sikunasinthe, zomwe zikutanthauza kuti ma NCO nanomaterials adawonetsa kusankhidwa kwabwino kwambiri pakuzindikira shuga mosasamala kanthu za kusiyana kwawo kwa morphological.Chithunzi S13 chikuwonetsa kukhazikika kwa ma NCO nanomatadium omwe amawunikidwa ndi mayankho a CA mu 0.1 M NaOH, pomwe glucose wa 1 mm adawonjezeredwa ku electrolyte kwa nthawi yayitali (80,000 s).Mayankho apano a UNCO, PNCO, TNCO, ndi FNCO anali 98.6%, 97.5%, 98.4%, ndi 96.8%, motero, poyambira pano ndikuwonjezera shuga wowonjezera wa 1 mM pambuyo pa 80,000 s.Zonse za NCO nanomatadium zimawonetsa kukhazikika kwa redox ndi mitundu ya shuga kwa nthawi yayitali.Makamaka, chizindikiro chamakono cha UNCO sichinangosunga 97.1% ya nthawi yake yoyamba, komanso kusunga morphology ndi mankhwala ogwirizana ndi mankhwala pambuyo poyesa kukhazikika kwa chilengedwe kwa masiku 7 (Zithunzi S14 ndi S15a).Kuonjezera apo, kubereka ndi kubereka kwa UNCO kunayesedwa monga momwe tawonetsera mkuyu S15b, c.Kuwerengeka kwa Relative Standard Deviation (RSD) kwa kubalana ndi kubwerezanso kunali 2.42% ndi 2.14%, motsatana, kuwonetsa zomwe zitha kugwiritsidwa ntchito ngati sensa ya glucose yamakampani.Izi zikuwonetsa kukhazikika kwamapangidwe ndi mankhwala a UNCO pansi pamikhalidwe ya oxidizing kuti azindikire shuga.
N'zoonekeratu kuti electrochemical ntchito NCO nanomaterials kwa shuga kudziwika makamaka zokhudzana ndi ubwino structural wa gawo loyamba lokonzedwa ndi njira hydrothermal ndi zina (mkuyu. S16).Malo okwera kwambiri a UNCO ali ndi malo opangira magetsi ambiri kuposa ma nanostructures ena, omwe amathandizira kusintha kachitidwe ka redox pakati pa zinthu zomwe zimagwira ntchito ndi tinthu tating'ono ta shuga.Mawonekedwe a mesoporous a UNCO amatha kuwulula malo ambiri a Ni ndi Co ku electrolyte kuti azindikire shuga, zomwe zimapangitsa kuti pakhale kuyankha mwachangu kwamagetsi.Ma nanowire a mbali imodzi ku UNCO atha kuonjezera kuchuluka kwa kufalikira popereka njira zazifupi zoyendera ma ma ion ndi ma electron.Chifukwa cha mawonekedwe apadera omwe atchulidwa pamwambapa, machitidwe a electrochemical a UNCO pozindikira shuga ndi apamwamba kuposa a PNCO, TNCO, ndi FNCO.Izi zikuwonetsa kuti mawonekedwe apadera a UNCO okhala ndi malo apamwamba kwambiri komanso kukula kwa pore amatha kupereka magwiridwe antchito abwino kwambiri a electrochemical pakuzindikira shuga.
Zotsatira za malo enieni pamtundu wa electrochemical wa NCO nanomaterials adaphunziridwa.NCO nanomatadium zokhala ndi malo osiyanasiyana apadera adapezedwa ndi njira yosavuta ya hydrothermal ndi zowonjezera zosiyanasiyana.Zina zowonjezera panthawi ya kaphatikizidwe zimalowa m'magulu osiyanasiyana a mankhwala ndikupanga magawo osiyanasiyana oyambirira.Izi zapangitsa kuti adziphatikizepo ma nanostructures osiyanasiyana okhala ndi ma morphologies ofanana ndi hedgehog, singano ya paini, tremella, ndi maluwa.Kutentha kotsatira pambuyo pake kumatsogolera ku chikhalidwe chofanana cha mankhwala a crystalline NCO nanomaterials ndi mapangidwe a spinel pamene akusunga morphology yawo yapadera.Kutengera ndi mawonekedwe amtundu wosiyanasiyana, magwiridwe antchito a electrochemical a NCO nanomatadium pozindikira shuga asintha kwambiri.Makamaka, mphamvu ya shuga ya NCO nanomatadium yokhala ndi ma urchin morphology yakula mpaka 116.33 µA mM-1 cm-2 yokhala ndi coefficient yolumikizana kwambiri (R2) ya 0.99 mu mzere wa 0.01-6 mm.Ntchitoyi ikhoza kupereka maziko asayansi a uinjiniya wa morphological kuti asinthe malo enaake ndikupititsa patsogolo magwiridwe antchito a electrochemical a non-enzymatic biosensor application.
Ni(NO3)2 6H2O, Co(NO3)2 6H2O, urea, hexamethylenetetramine (HMT), ammonium fluoride (NH4F), sodium hydroxide (NaOH), d-(+)-glucose, lactic acid (LA), dopamine hydrochloride ( DA), L-ascorbic acid (AA) ndi uric acid (UA) adagulidwa ku Sigma-Aldrich.Ma reagents onse omwe amagwiritsidwa ntchito anali a kalasi yowunikira ndipo adagwiritsidwa ntchito popanda kuyeretsedwa kwina.
NiCo2O4 idapangidwa ndi njira yosavuta ya hydrothermal yotsatiridwa ndi chithandizo cha kutentha.Mwachidule: 1 mmol wa nickel nitrate (Ni(NO3)2∙6H2O) ndi 2 mmol wa cobalt nitrate (Co(NO3)2∙6H2O) anasungunuka mu 30 ml ya madzi osungunuka.Pofuna kuwongolera morphology ya NiCo2O4, zowonjezera monga urea, ammonium fluoride ndi hexamethylenetetramine (HMT) zidawonjezeredwa ku yankho lomwe lili pamwambapa.Chosakaniza chonsecho chinasamutsidwa ku 50 ml ya Teflon-lined autoclave ndi kugonjetsedwa ndi hydrothermal reaction mu uvuni wa convection pa 120 ° C. kwa maola 6.Pambuyo pa kuzirala kwachilengedwe mpaka kutentha kwa chipinda, mpweya wotsatirawo udapangidwa ndi centrifuged ndikutsukidwa kangapo ndi madzi osungunuka ndi ethanol, kenako kuumitsa usiku wonse pa 60 ° C.Pambuyo pake, zitsanzo zokonzedwa mwatsopano zimatenthedwa pa 400 ° C kwa maola 4 mumlengalenga.Tsatanetsatane wa zoyeserera zalembedwa mu Supplementary Information Table S2.
X-ray diffraction analysis (XRD, X'Pert-Pro MPD; PANalytical) inkagwiritsidwa ntchito pogwiritsa ntchito ma radiation a Cu-Kα (λ = 0.15418 nm) pa 40 kV ndi 30 mA kuti aphunzire kapangidwe kazinthu zonse za NCO nanomaterials.Njira zosinthira zidalembedwa m'makona a 2θ 10-80 ° ndi sitepe ya 0.05 °.Surface morphology ndi microstructure zidawunikiridwa pogwiritsa ntchito kuwunika kwa ma electron microscopy (FESEM; Nova SEM 200, FEI) ndi scanning transmission electron microscopy (STEM; TALOS F200X, FEI) yokhala ndi ma X-ray spectroscopy (EDS).Malo a valence pamtunda adawunikidwa ndi X-ray photoelectron spectroscopy (XPS; PHI 5000 Versa Probe II, ULVAC PHI) pogwiritsa ntchito ma radiation a Al Kα (hν = 1486.6 eV).Mphamvu zomangirira zidasinthidwa pogwiritsa ntchito nsonga ya C 1 pa 284.6 eV monga chofotokozera.Pambuyo pokonza zitsanzo pa tinthu ta KBr, mawonekedwe a Fourier akusintha mawonekedwe a infuraredi (FT-IR) adalembedwa mumtundu wa wavenumber 1500-400 cm-1 pa spectrometer ya Jasco-FTIR-6300.Zowonera za Raman zidapezedwanso pogwiritsa ntchito chowonera cha Raman (Horiba Co., Japan) chokhala ndi laser ya He-Ne (632.8 nm) ngati gwero losangalatsa.Brunauer-Emmett-Teller (BET; BELSORP mini II, MicrotracBEL, Corp.) adagwiritsa ntchito BELSORP mini II analyzer (MicrotracBEL Corp.) kuti ayese kutentha kwapansi kwa N2 adsorption-desorption isotherms kuti ayese malo enieni komanso kukula kwa pore.
Miyezo yonse ya electrochemical, monga cyclic voltammetry (CV) ndi chronoamperometry (CA), inachitidwa pa PGSTAT302N potentiostat (Metrohm-Autolab) pa kutentha kwa chipinda pogwiritsa ntchito makina atatu a electrode mu 0.1 M NaOH yankho lamadzi.Elekitirodi yogwira ntchito yozikidwa pa magalasi opangira ma electrode agalasi (GC), elekitirodi ya Ag/AgCl, ndi mbale ya pulatinamu zinagwiritsidwa ntchito ngati ma elekitirodi ogwirira ntchito, maelekitirodi owerengera, ndi ma elekitirodi owerengera, motsatana.Ma CV adalembedwa pakati pa 0 ndi 0.6 V pamasinthidwe osiyanasiyana a 5-100 mV s-1.Kuyeza ECSA, CV idachitidwa mumitundu ya 0.1-0.2 V pamitundu yosiyanasiyana ya sikani (5-100 mV s-1).Pezani sampuli ya CA reaction ya glucose pa 0.5 V ndikugwedeza.Kuti muyeze kukhudzika ndi kusankha, gwiritsani ntchito shuga wa 0.01–6 mM, 0.1 mM LA, DA, AA, ndi UA mu 0.1 M NaOH.Kuchulukitsa kwa UNCO kunayesedwa pogwiritsa ntchito maelekitirodi atatu osiyanasiyana ophatikizidwa ndi shuga wa 5 mM pansi pamikhalidwe yabwino.Kubwerezanso kudawunikidwanso popanga miyeso itatu ndi electrode imodzi ya UNCO mkati mwa maola 6.
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