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Peb tshawb xyuas cov txiaj ntsig ntawm thaj chaw tshwj xeeb ntawm cov khoom siv hluav taws xob ntawm NiCo2O4 (NCO) rau kev kuaj ntshav qabzib.NCO nanomaterials nrog kev tswj xyuas thaj chaw tshwj xeeb tau tsim los ntawm hydrothermal synthesis nrog additives, thiab nws tus kheej-assembling nanostructures nrog hedgehog, Pine koob, tremella thiab paj zoo li morphology kuj tau tsim.Lub novelty ntawm txoj kev no yog nyob rau hauv lub systematic tswj ntawm cov tshuaj tiv thaiv txoj kev los ntawm kev ntxiv ntau yam additives thaum lub sij hawm synthesis, uas ua rau lub spontaneous tsim ntawm ntau yam morphologies yam tsis muaj qhov sib txawv ntawm cov qauv siv lead ua thiab tshuaj lom neeg lub xeev ntawm cov ntsiab lus.Qhov kev tswj morphological ntawm NCO nanomaterials ua rau muaj kev hloov pauv tseem ceeb hauv electrochemical kev ua tau zoo ntawm kev kuaj ntshav qabzib.Ua ke nrog cov khoom ua cim, kev sib raug zoo ntawm thaj chaw tshwj xeeb thiab kev ua haujlwm ntawm electrochemical rau kev kuaj ntshav qabzib tau tham.Txoj haujlwm no tuaj yeem muab kev nkag siab txog kev tshawb fawb rau thaj tsam thaj chaw tuning ntawm nanostructures uas txiav txim siab lawv txoj haujlwm rau cov ntawv thov hauv cov piam thaj biosensors.
Cov ntshav qabzib hauv cov ntshav muab cov ntaub ntawv tseem ceeb txog cov metabolism thiab lub cev lub cev ntawm lub cev 1,2.Piv txwv li, qhov txawv txav ntawm cov piam thaj hauv lub cev tuaj yeem yog qhov tseem ceeb ntawm cov teeb meem kev noj qab haus huv, suav nrog ntshav qab zib, kab mob plawv, thiab rog rog3,4,5.Yog li ntawd, kev saib xyuas cov ntshav qab zib tsis tu ncua yog ib qho tseem ceeb heev rau kev noj qab haus huv zoo.Txawm hais tias muaj ntau hom glucose sensors uas siv physicochemical kuaj pom tau raug tshaj tawm, tsis tshua muaj rhiab heev thiab lub sij hawm teb qeeb tseem cuam tshuam rau kev soj ntsuam cov piam thaj tas li 6,7,8.Tsis tas li ntawd, tam sim no nrov electrochemical glucose sensors raws li cov tshuaj tiv thaiv enzymatic tseem muaj qee qhov kev txwv txawm tias lawv qhov zoo ntawm cov lus teb ceev ceev, siab rhiab heev thiab cov txheej txheem tsim yooj yim 9,10.Yog li ntawd, ntau hom non-enzymatic electrochemical sensors tau kawm ntau yam los tiv thaiv enzyme denaturation thaum tswj qhov zoo ntawm electrochemical biosensors9,11,12,13.
Transition metal compounds (TMCs) muaj cov kev ua haujlwm siab catalytic txaus nrog rau cov piam thaj, uas nthuav dav lawv cov ntawv thov hauv electrochemical glucose sensors13,14,15.Txog tam sim no, ntau yam kev tsim qauv tsim nyog thiab txoj hauv kev yooj yim rau kev sib txuas ntawm TMS tau raug npaj los txhim kho qhov rhiab heev, xaiv, thiab electrochemical stability ntawm glucose detection16,17,18.Piv txwv li, tsis muaj kev hloov pauv hlau oxides xws li tooj liab oxide (CuO) 11,19, zinc oxide (ZnO) 20, nickel oxide (NiO) 21,22, cobalt oxide (Co3O4) 23,24 thiab cerium oxide (CeO2) 25 yog electrochemically active nrog rau cov piam thaj.Kev nce qib tsis ntev los no hauv binary hlau oxides xws li npib tsib xee cobaltate (NiCo2O4) rau kev kuaj ntshav qabzib tau pom tias muaj kev sib koom ua ke ntxiv ntawm cov khoom siv hluav taws xob ntau ntxiv 26,27,28,29,30.Hauv particular, cov muaj pes tsawg leeg thiab morphology tswj los tsim TMS nrog ntau yam nanostructures tuaj yeem ua kom pom kev zoo dua vim lawv qhov chaw loj, yog li nws tau pom zoo kom tsim morphology tswj TMS rau kev txhim kho cov piam thaj 20,25,30,31,32, 33.34, 35 ib.
Ntawm no peb qhia NiCo2O4 (NCO) nanomaterials nrog txawv morphologies rau kev kuaj ntshav qabzib.NCO nanomaterials yog tau los ntawm ib tug yooj yim hydrothermal txoj kev siv ntau yam additives, tshuaj additives yog ib tug ntawm cov tseem ceeb yam tseem ceeb nyob rau hauv lub self-assembly ntawm nanostructures ntawm ntau yam morphologies.Peb tau tshawb xyuas cov txiaj ntsig ntawm NCOs nrog cov qauv sib txawv ntawm lawv cov kev ua haujlwm electrochemical rau kev kuaj ntshav qabzib, suav nrog rhiab heev, xaiv, txwv tsis pub kuaj pom, thiab kev ruaj ntseg mus ntev.
Peb muab cov ntaub ntawv NCO nanomaterials (abbreviated UNCO, PNCO, TNCO thiab FNCO raws) nrog microstructures zoo ib yam li hiav txwv urchins, ntoo thuv koob, tremella thiab paj.Daim duab 1 qhia txog kev sib txawv ntawm UNCO, PNCO, TNCO, thiab FNCO.SEM cov duab thiab EDS cov duab qhia tau hais tias Ni, Co, thiab O tau sib npaug ntawm cov khoom siv NCO nanomaterials, raws li pom hauv daim duab 1 thiab 2. S1 thiab S2, raws li.Ntawm daim duab.2a,b qhia cov neeg sawv cev TEM cov duab ntawm NCO nanomaterials nrog txawv morphology.UNCO yog ib lub microsphere ntawm tus kheej (inch: ~ 5 µm) muaj li ntawm nanowires nrog NCO nanoparticles (qhov nruab nrab particle loj: 20 nm).Qhov tshwj xeeb microstructure no xav kom muab thaj chaw loj los pab txhawb electrolyte diffusion thiab electron thauj.Qhov sib ntxiv ntawm NH4F thiab urea thaum lub sij hawm synthesis ua rau lub thicker acicular microstructure (PNCO) 3 µm ntev thiab 60 nm dav, muaj li ntawm nanoparticles loj.Qhov sib ntxiv ntawm HMT es tsis txhob NH4F ua rau muaj qhov zoo li tremello morphology (TNCO) nrog wrinkled nanosheets.Kev taw qhia ntawm NH4F thiab HMT thaum lub sijhawm sib txuas ua rau kev sib sau ua ke ntawm cov ntaub ntawv uas nyob ib sab wrinkled, uas ua rau lub paj zoo li morphology (FNCO).Daim duab HREM (Fig. 2c) qhia qhov sib txawv grating bands nrog interplanar spacings ntawm 0.473, 0.278, 0.50, thiab 0.237 nm, sib xws rau (111), (220), (311), thiab (222) NiCo2O4 dav hlau, s .Xaiv thaj tsam electron diffraction pattern (SAED) ntawm NCO nanomaterials (inset to Fig. 2b) kuj tau lees paub qhov polycrystalline xwm ntawm NiCo2O4.Cov txiaj ntsig ntawm high-angle annular dark imaging (HAADF) thiab EDS mapping qhia tias tag nrho cov ntsiab lus sib npaug sib npaug hauv NCO nanomaterial, raws li qhia hauv daim duab 2d.
Schematic illustration ntawm tus txheej txheem ntawm tsim ntawm NiCo2O4 nanostructures nrog tswj morphology.Schematics thiab SEM cov duab ntawm ntau yam nanostructures kuj pom.
Morphological and structural characterization of NCO nanomaterials: (a) TEM image, (b) TEM image along with SAED pattern, (c) grating-resolved HRTEM image and corresponding HADDF images of Ni, Co, and O in (d) NCO nanomaterials..
X-ray diffraction qauv ntawm NCO nanomaterials ntawm ntau yam morphologies yog qhia nyob rau hauv daim duab.3 ib a.Lub diffraction peaks ntawm 18.9, 31.1, 36.6, 44.6, 59.1 thiab 64.9 ° qhia lub dav hlau (111), (220), (311), (400), (511) thiab (440) NiCo2O4, raws li, uas muaj ib tug cubic. spinel structure (JCPDS No. 20-0781) 36. The FT-IR spectra of the NCO nanomaterials are shown in Fig.3b ib.Ob lub zog vibrational bands nyob rau hauv cheeb tsam ntawm 555 thiab 669 cm-1 sib haum mus rau metallic (Ni thiab Co) oxygen rub los ntawm tetrahedral thiab octahedral txoj hauj lwm ntawm NiCo2O437 spinel, feem.Txhawm rau kom nkag siab zoo dua cov yam ntxwv ntawm NCO nanomaterials, Raman spectra tau txais raws li qhia hauv daim duab 3c.Plaub lub ncov pom ntawm 180, 459, 503, thiab 642 cm-1 sib haum rau Raman hom F2g, E2g, F2g, thiab A1g ntawm NiCo2O4 spinel, feem.XPS ntsuas tau ua los txiav txim siab qhov chaw tshuaj lom neeg lub xeev ntawm cov khoom hauv NCO nanomaterials.Ntawm daim duab.3d qhia XPS spectrum ntawm UNCO.Lub spectrum ntawm Ni 2p muaj ob lub ntsiab ncov nyob rau ntawm kev sib txuas ntawm lub zog ntawm 854.8 thiab 872.3 eV, sib xws rau Ni 2p3/2 thiab Ni 2p1/2, thiab ob lub vibrational satellites ntawm 860.6 thiab 879.1 eV, raws li.Qhov no qhia tias muaj Ni2+ thiab Ni3+ oxidation xeev hauv NCO.Peaks nyob ib ncig ntawm 855.9 thiab 873.4 eV yog rau Ni3+, thiab peaks nyob ib ncig ntawm 854.2 thiab 871.6 eV yog rau Ni2+.Ib yam li ntawd, Co2p spectrum ntawm ob lub voj voog sib txuas qhia pom cov yam ntxwv siab tshaj plaws rau Co2 + thiab Co3 + ntawm 780.4 (Co 2p3/2) thiab 795.7 eV (Co 2p1/2).Peaks ntawm 796.0 thiab 780.3 eV sib haum rau Co2+, thiab peaks ntawm 794.4 thiab 779.3 eV sib haum rau Co3+.Nws yuav tsum raug sau tseg tias lub xeev polyvalent ntawm cov hlau ions (Ni2 + / Ni3 + thiab Co2 + / Co3 +) hauv NiCo2O4 txhawb kev nce hauv electrochemical kev ua 37,38.Ni2p thiab Co2p spectra rau UNCO, PNCO, TNCO, thiab FNCO pom cov txiaj ntsig zoo sib xws, raws li qhia hauv daim duab.S3.Tsis tas li ntawd, O1s spectra ntawm tag nrho NCO nanomaterials (Fig. S4) pom ob peaks ntawm 592.4 thiab 531.2 eV, uas tau txuam nrog cov hlau-oxygen thiab oxygen bonds nyob rau hauv cov hydroxyl pawg ntawm NCO nto, feem 39.Txawm hais tias cov qauv ntawm NCO nanomaterials zoo sib xws, qhov sib txawv ntawm cov morphological hauv cov additives qhia tias txhua tus additive tuaj yeem koom nrog qhov sib txawv ntawm cov tshuaj lom neeg los tsim NCO.Qhov no tswj lub zog zoo nucleation thiab grain loj hlob cov kauj ruam, yog li tswj particle loj thiab degree ntawm agglomeration.Yog li, kev tswj hwm ntawm ntau yam txheej txheem, suav nrog cov khoom siv ntxiv, cov tshuaj tiv thaiv lub sijhawm, thiab qhov kub thiab txias thaum lub sijhawm sib xyaw, tuaj yeem siv los tsim cov microstructure thiab txhim kho electrochemical kev ua tau zoo ntawm NCO nanomaterials rau kev kuaj ntshav qabzib.
(a) X-ray diffraction patterns, (b) FTIR and (c) Raman spectra of NCO nanomaterials, (d) XPS spectra of Ni 2p and Co 2p from UNCO.
Lub morphology ntawm adapted NCO nanomaterials yog ze ze rau kev tsim ntawm thawj theem tau los ntawm ntau yam additives depicted nyob rau hauv daim duab S5.Tsis tas li ntawd, X-ray thiab Raman spectra ntawm cov qauv npaj tshiab (Figures S6 thiab S7a) tau pom tias kev koom tes ntawm cov tshuaj sib txawv ntawm cov tshuaj ntxiv ua rau muaj qhov sib txawv crystallographic: Ni thiab Co carbonate hydroxides tau pom nyob rau hauv hiav txwv urchins thiab Pine koob qauv, thaum raws li Cov qauv hauv daim ntawv ntawm tremella thiab paj qhia tias muaj cov nickel thiab cobalt hydroxides.FT-IR thiab XPS spectra ntawm cov qauv npaj tau pom nyob rau hauv daim duab 1 thiab 2. S7b-S9 kuj muab pov thawj tseeb ntawm qhov sib txawv crystallographic tau hais los saum no.Los ntawm cov khoom siv ntawm cov qauv npaj, nws pom tseeb tias cov tshuaj ntxiv tau koom nrog cov tshuaj tiv thaiv hydrothermal thiab muab cov txheej txheem sib txawv kom tau txais cov theem pib nrog cov morphologies sib txawv40,41,42.Kev sib dhos ntawm tus kheej ntawm cov morphologies sib txawv, muaj xws li ib-dimensional (1D) nanowires thiab ob-dimensional (2D) nanosheets, tau piav qhia los ntawm cov tshuaj sib txawv ntawm cov theem pib (Ni thiab Co ions, nrog rau cov pab pawg ua haujlwm), ua raws li siv lead ua kev loj hlob42, 43, 44, 45, 46, 47. Thaum lub sij hawm tom qab thermal ua, ntau theem pib hloov mus rau NCO spinel thaum tuav lawv cov cim morphology, raws li qhia hauv daim duab 1 thiab 2. 2 thiab 3a.
Morphological sib txawv hauv NCO nanomaterials tuaj yeem cuam tshuam rau thaj chaw electrochemically active deg rau kev kuaj ntshav qabzib, yog li txiav txim siab tag nrho electrochemical yam ntxwv ntawm cov piam thaj sensor.N2 BET adsorption-desorption isotherm yog siv los kwv yees qhov pore loj thiab thaj chaw tshwj xeeb ntawm NCO nanomaterials.Ntawm daim duab.4 qhia BET isotherms ntawm ntau yam NCO nanomaterials.Qhov BET tshwj xeeb thaj chaw rau UNCO, PNCO, TNCO thiab FNCO tau kwv yees ntawm 45.303, 43.304, 38.861 thiab 27.260 m2 / g, raws li.UNCO muaj qhov siab tshaj plaws BET nto thaj tsam (45.303 m2 g-1) thiab qhov loj tshaj plaws pore ntim (0.2849 cm3 g-1), thiab qhov pore loj faib yog nqaim.Cov txiaj ntsig BET rau NCO nanomaterials tau qhia hauv Table 1. N2 adsorption-desorption curves zoo ib yam li hom IV isothermal hysteresis loops, qhia tias tag nrho cov qauv muaj cov qauv mesoporous48.Mesoporous UNCOs nrog thaj chaw siab tshaj plaws thiab qhov pore ntim siab tshaj plaws yuav tsum muab ntau qhov chaw ua haujlwm rau cov tshuaj tiv thaiv redox, ua rau kev txhim kho electrochemical kev ua tau zoo.
BET cov txiaj ntsig rau (a) UNCO, (b) PNCO, (c) TNCO, thiab (d) FNCO.Lub inset qhia qhov sib thooj pore loj faib.
Lub electrochemical redox cov tshuaj tiv thaiv ntawm NCO nanomaterials nrog ntau yam morphologies rau kev kuaj ntshav qabzib tau raug soj ntsuam siv CV ntsuas.Ntawm daim duab.5 qhia CV curves ntawm NCO nanomaterials hauv 0.1 M NaOH alkaline electrolyte nrog thiab tsis muaj 5 mM qabzib ntawm tus nqi scan ntawm 50 mVs-1.Thaum tsis muaj qabzib, redox peaks tau pom ntawm 0.50 thiab 0.35 V, sib haum rau oxidation txuam nrog M-O (M: Ni2+, Co2+) thiab M*-O-OH (M*: Ni3+, Co3+).siv OH anion.Tom qab qhov sib ntxiv ntawm 5 mM qabzib, cov tshuaj tiv thaiv redox nyob rau saum npoo ntawm NCO nanomaterials tau nce ntxiv, uas tej zaum yuav yog vim oxidation ntawm qabzib rau gluconolactone.Daim duab S10 qhia txog lub ncov redox tam sim no ntawm scan nqi ntawm 5-100 mV s-1 hauv 0.1 M NaOH tov.Nws yog tseeb hais tias lub ncov redox tam sim no nce nrog nce tus nqi scan, qhia tias NCO nanomaterials muaj xws li diffusion tswj electrochemical cwj pwm50,51.Raws li pom hauv daim duab S11, thaj tsam electrochemical deg (ECSA) ntawm UNCO, PNCO, TNCO, thiab FNCO yog kwv yees li 2.15, 1.47, 1.2, thiab 1.03 cm2, raws li.Qhov no qhia tias UNCO muaj txiaj ntsig zoo rau cov txheej txheem electrocatalytic, ua kom yooj yim rau kev tshawb nrhiav cov piam thaj.
CV curves ntawm (a) UNCO, (b) PNCO, (c) TNCO, thiab (d) FNCO electrodes tsis muaj piam thaj thiab ntxiv nrog 5 mM qabzib ntawm tus nqi scan ntawm 50 mVs-1.
Electrochemical kev ua tau zoo ntawm NCO nanomaterials rau kev kuaj ntshav qabzib tau raug tshawb xyuas thiab cov txiaj ntsig tau pom hauv daim duab 6. Glucose rhiab heev yog txiav txim siab los ntawm CA txoj kev los ntawm kev ntxiv ntau yam ntawm cov piam thaj (0.01–6 mM) hauv 0.1 M NaOH kua ntawm 0.5. V nrog lub sijhawm ntawm 60s.Raws li qhia hauv daim duab.6a–d, NCO nanomaterials qhia txawv rhiab heev ntawm 84.72 mus rau 116.33 µA mM-1 cm-2 nrog high correlation coefficients (R2) los ntawm 0.99 txog 0.993.Lub calibration nkhaus ntawm qabzib concentration thiab cov tshuaj tiv thaiv tam sim no ntawm NCO nanomaterials yog qhia nyob rau hauv daim duab.S12.Cov kev txwv ntawm kev kuaj pom (LOD) ntawm NCO nanomaterials nyob hauv thaj tsam ntawm 0.0623–0.0783 µM.Raws li cov txiaj ntsig ntawm CA kev xeem, UNCO pom qhov siab tshaj plaws rhiab heev (116.33 μA mM-1 cm-2) nyob rau hauv ntau qhov kev tshawb pom.Qhov no tuaj yeem piav qhia los ntawm nws qhov tshwj xeeb hauv hiav txwv urchin-zoo li morphology, muaj cov qauv mesoporous nrog thaj chaw loj tshwj xeeb uas muab ntau qhov chaw ua haujlwm rau cov hom qabzib.Kev ua tau zoo electrochemical ntawm NCO nanomaterials nthuav tawm hauv Table S1 lees paub qhov zoo tshaj plaws electrochemical glucose detection kev ua tau zoo ntawm NCO nanomaterials npaj rau hauv txoj kev tshawb no.
CA cov lus teb ntawm UNCO (a), PNCO (b), TNCO (c), thiab FNCO (d) electrodes nrog qabzib ntxiv rau 0.1 M NaOH tov ntawm 0.50 V. Cov insets qhia calibration curves ntawm cov lus teb tam sim no ntawm NCO nanomaterials: (e ) KA cov lus teb ntawm UNCO, (f) PNCO, (g) TNCO, thiab (h) FNCO nrog stepwise ntxiv ntawm 1 mM qabzib thiab 0.1 mM cuam tshuam cov tshuaj (LA, DA, AA, thiab UA).
Lub peev xwm los tiv thaiv kev cuam tshuam ntawm kev kuaj ntshav qabzib yog lwm qhov tseem ceeb hauv kev xaiv thiab ntsuas cov piam thaj los ntawm kev cuam tshuam cov tebchaw.Ntawm daim duab.6e–h qhia lub peev xwm tiv thaiv kev cuam tshuam ntawm NCO nanomaterials hauv 0.1 M NaOH tov.Feem ntau cuam tshuam cov molecules xws li LA, DA, AA thiab UA raug xaiv thiab ntxiv rau cov electrolyte.Cov lus teb tam sim no ntawm NCO nanomaterials rau cov piam thaj yog pom tseeb.Txawm li cas los xij, cov lus teb tam sim no rau UA, DA, AA thiab LA tsis hloov pauv, uas txhais tau hais tias NCO nanomaterials tau pom zoo xaiv rau kev kuaj ntshav qabzib tsis hais lawv qhov sib txawv ntawm morphological.Daim duab S13 qhia txog kev ruaj ntseg ntawm NCO nanomaterials tshuaj xyuas los ntawm CA teb nyob rau hauv 0.1 M NaOH, qhov twg 1 mM qabzib tau ntxiv rau cov electrolyte ntev (80,000 s).Cov lus teb tam sim no ntawm UNCO, PNCO, TNCO, thiab FNCO yog 98.6%, 97.5%, 98.4%, thiab 96.8%, feem, ntawm qhov pib tam sim no nrog ntxiv ntawm 1 mM qabzib ntxiv tom qab 80,000 s.Tag nrho cov NCO nanomaterials muaj cov tshuaj tiv thaiv redox ruaj khov nrog cov piam thaj hauv lub sijhawm ntev.Tshwj xeeb, UNCO cov teeb liab tam sim no tsis tsuas yog khaws cia 97.1% ntawm nws qhov pib tam sim no, tab sis tseem khaws nws cov morphology thiab tshuaj lom neeg daim ntawv cog lus tom qab 7-hnub ib puag ncig kev ruaj ntseg mus sij hawm ntev (Figures S14 thiab S15a).Tsis tas li ntawd, qhov kev tsim tawm thiab rov tsim dua tshiab ntawm UNCO tau raug sim raws li qhia hauv daim duab S15b, c.Qhov ntsuas txheeb ze tus qauv sib txawv (RSD) ntawm kev rov ua dua thiab rov ua dua yog 2.42% thiab 2.14%, feem, qhia tias muaj peev xwm siv tau raws li qib qib qib qabzib.Qhov no qhia txog cov qauv zoo heev thiab tshuaj lom neeg ruaj khov ntawm UNCO nyob rau hauv oxidizing tej yam kev mob rau kev kuaj ntshav qabzib.
Nws yog qhov tseeb tias kev ua haujlwm ntawm electrochemical ntawm NCO nanomaterials rau kev kuaj ntshav qabzib feem ntau yog cuam tshuam nrog cov qauv zoo ntawm thawj theem npaj los ntawm txoj kev hydrothermal nrog additives (Fig. S16).Qhov chaw siab saum npoo UNCO muaj ntau qhov chaw electroactive dua li lwm cov nanostructures, uas pab txhim kho cov tshuaj tiv thaiv redox ntawm cov khoom nquag thiab cov piam thaj.Cov qauv mesoporous ntawm UNCO tuaj yeem yooj yim nthuav tawm ntau qhov chaw Ni thiab Co rau cov electrolyte kom kuaj tau cov piam thaj, ua rau cov lus teb ceev ceev electrochemical.Ib-dimensional nanowires nyob rau hauv UNCO tuaj yeem ua rau kom muaj qhov sib txawv ntxiv los ntawm kev muab txoj hauv kev luv luv rau ions thiab electrons.Vim muaj cov yam ntxwv tshwj xeeb uas tau hais los saum no, kev ua haujlwm ntawm electrochemical ntawm UNCO rau kev kuaj ntshav qabzib zoo dua li ntawm PNCO, TNCO, thiab FNCO.Qhov no qhia tau hais tias UNCO morphology tshwj xeeb nrog thaj chaw siab tshaj plaws thiab qhov pore loj tuaj yeem muab cov tshuaj electrochemical zoo rau kev kuaj ntshav qabzib.
Cov txiaj ntsig ntawm thaj chaw tshwj xeeb ntawm cov yam ntxwv electrochemical ntawm NCO nanomaterials tau kawm.NCO nanomaterials nrog qhov sib txawv ntawm thaj chaw tshwj xeeb tau txais los ntawm txoj kev yooj yim hydrothermal thiab ntau yam khoom ntxiv.Cov additives sib txawv thaum lub sij hawm synthesis nkag mus rau hauv cov tshuaj sib txawv thiab tsim cov theem pib sib txawv.Qhov no tau ua rau nws tus kheej ua ke ntawm ntau yam nanostructures nrog morphologies zoo ib yam li hedgehog, ntoo thuv koob, tremella, thiab paj.Tom qab cua sov tom qab ua rau muaj cov tshuaj zoo sib xws ntawm crystalline NCO nanomaterials nrog cov qauv spinel thaum tuav lawv cov morphology tshwj xeeb.Nyob ntawm thaj tsam ntawm qhov sib txawv morphology, electrochemical kev ua tau zoo ntawm NCO nanomaterials rau kev kuaj ntshav qabzib tau zoo heev.Tshwj xeeb, cov piam thaj rhiab heev ntawm NCO nanomaterials nrog hiav txwv urchin morphology tau nce mus rau 116.33 µA mM-1 cm-2 nrog kev sib raug zoo coefficient (R2) ntawm 0.99 hauv linear ntau ntawm 0.01-6 mM.Txoj haujlwm no tuaj yeem muab lub hauv paus rau kev tshawb fawb txog kev tsim vaj tsev morphological los kho thaj chaw tshwj xeeb thiab txhim kho cov khoom siv hluav taws xob ntxiv ntawm cov ntawv siv tsis-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 ( DA), L-ascorbic acid (AA) thiab uric acid (UA) tau yuav los ntawm Sigma-Aldrich.Tag nrho cov reagents uas siv tau yog qib analytical thiab tau siv yam tsis muaj purification ntxiv.
NiCo2O4 tau tsim los ntawm txoj kev yooj yim hydrothermal ua raws li kev kho cua sov.Luv luv: 1 mmol ntawm nickel nitrate (Ni (NO3) 2∙6H2O) thiab 2 mmol ntawm cobalt nitrate (Co (NO3) 2∙6H2O) tau yaj hauv 30 ml ntawm dej distilled.Txhawm rau tswj cov morphology ntawm NiCo2O4, cov tshuaj ntxiv xws li urea, ammonium fluoride thiab hexamethylenetetramine (HMT) tau xaiv ntxiv rau cov tshuaj saum toj no.Tom qab ntawd tag nrho cov sib tov tau pauv mus rau 50 ml Teflon-lined autoclave thiab raug rau cov tshuaj tiv thaiv hydrothermal hauv qhov cub convection ntawm 120 ° C. rau 6 teev.Tom qab ntuj txias rau hauv chav tsev kub, lub resulting precipitate yog centrifuged thiab ntxuav ob peb zaug nrog distilled dej thiab ethanol, thiab ces qhuav ib hmos ntawm 60 ° C.Tom qab ntawd, cov qauv tshiab tau npaj tau calcined ntawm 400 ° C rau 4 teev nyob rau hauv huab cua.Cov ntsiab lus ntawm cov kev sim tau teev nyob rau hauv Daim Ntawv Qhia Ntxiv S2.
X-ray diffraction tsom xam (XRD, X'Pert-Pro MPD; PANalytical) tau ua los ntawm Cu-Kα hluav taws xob (λ = 0.15418 nm) ntawm 40 kV thiab 30 mA los kawm txog cov yam ntxwv ntawm tag nrho NCO nanomaterials.Diffraction qauv tau sau tseg nyob rau hauv qhov ntau ntawm cov ces kaum 2θ 10-80 ° nrog ib kauj ruam ntawm 0.05 °.Surface morphology thiab microstructure raug tshuaj xyuas siv teb emission scanning electron microscopy (FESEM; Nova SEM 200, FEI) thiab scanning kis electron microscopy (STEM; TALOS F200X, FEI) nrog lub zog dispersive X-ray spectroscopy (EDS).Lub valence xeev ntawm qhov chaw tau soj ntsuam los ntawm X-ray photoelectron spectroscopy (XPS; PHI 5000 Versa Probe II, ULVAC PHI) siv Al Kα hluav taws xob (hν = 1486.6 eV).Lub zog khi tau raug ntsuas siv C 1 s ncov ntawm 284.6 eV raws li kev siv.Tom qab npaj cov qauv ntawm KBr hais, Fourier transform infrared (FT-IR) spectra tau sau tseg hauv wavenumber range 1500-400 cm-1 ntawm Jasco-FTIR-6300 spectrometer.Raman spectra kuj tau siv lub Raman spectrometer (Horiba Co., Nyiv) nrog He-Ne laser (632.8 nm) ua qhov zoo siab.Brunauer-Emmett-Teller (BET; BELSORP mini II, MicrotracBEL, Corp.) tau siv BELSORP mini II analyzer (MicrotracBEL Corp.) los ntsuas qhov kub thiab txias N2 adsorption-desorption isotherms los kwv yees thaj chaw tshwj xeeb thiab qhov pore loj faib.
Tag nrho cov kev ntsuas electrochemical, xws li cyclic voltammetry (CV) thiab chronoamperometry (CA), tau ua ntawm PGSTAT302N potentiostat (Metrohm-Autolab) ntawm chav tsev kub uas siv peb-electrode system hauv 0.1 M NaOH aqueous tov.Ib qho electrode ua haujlwm raws li lub iav carbon electrode (GC), Ag / AgCl electrode, thiab platinum phaj tau siv los ua haujlwm electrode, siv electrode, thiab counter electrode, raws li.CVs tau kaw ntawm 0 thiab 0.6 V ntawm ntau qhov ntsuas ntawm 5-100 mV s-1.Txhawm rau ntsuas ECSA, CV tau ua nyob rau hauv thaj tsam ntawm 0.1-0.2 V ntawm ntau qhov ntsuas ntsuas (5-100 mV s-1).Tau cov qauv CA cov tshuaj tiv thaiv rau cov piam thaj ntawm 0.5 V nrog nplawm.Txhawm rau ntsuas rhiab heev thiab xaiv, siv 0.01–6 mM qabzib, 0.1 mM LA, DA, AA, thiab UA hauv 0.1 M NaOH.Kev rov tsim dua tshiab ntawm UNCO tau sim siv peb qhov sib txawv electrodes ntxiv nrog 5 mM qabzib nyob rau hauv cov xwm txheej zoo.Qhov rov ua dua tau raug kuaj xyuas los ntawm kev ntsuas peb zaug nrog ib qho UNCO electrode hauv 6 teev.
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