Wet Chemical Synthesis ine Additives Kudzora Nickel Cobaltate Surface Area yeGlucose Detection.

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Isu takaongorora mabatiro eiyo chaiyo nzvimbo pane electrochemical zvimiro zveNiCo2O4 (NCO) yekuona glucose.NCO nanomaterials ine inodzorwa yakananga nzvimbo yakagadzirwa ne hydrothermal synthesis ine additives, uye yekuzvibatanidza nanostructures ine hedgehog, pine tsono, tremella uye maruva senge morphology akagadzirwa zvakare.Hunhu hutsva hweiyi nzira huri mukutonga kwakarongeka kwekemikari yekuita nzira nekuwedzera zvakasiyana-siyana zvekuwedzera panguva yekubatanidza, izvo zvinotungamira mukungoitika kwega kweakasiyana morphologies pasina misiyano muchimiro chekristaro uye chimiro chemakemikari yezvinhu zvinoumbwa.Iyi morphological control yeNCO nanomaterials inotungamira kune shanduko huru mukuita kwe electrochemical yekuonekwa kweglucose.Mukubatana nehunhu hwezvinhu, hukama pakati peiyo nzvimbo yepasi uye electrochemical performance yekuonekwa kweglucose yakakurukurwa.Iri basa rinogona kupa nzwisiso yesainzi pamusoro penzvimbo yekugadzirisa nanostructures iyo inotaridza mashandiro adzo kune zvingangoita maapplication mune glucose biosensors.
Mazinga eglucose eropa anopa ruzivo rwakakosha nezve metabolic uye physiological mamiriro emuviri1,2.Semuenzaniso, mazinga asina kujairika eglucose mumuviri anogona kuve chiratidzo chakakosha chematambudziko akakomba ehutano, kusanganisira chirwere cheshuga, chirwere chemoyo, uye kufutisa3,4,5.Nokudaro, kugara uchitarisa mazinga ehuga eropa kwakakosha zvikuru pakuchengetedza hutano hwakanaka.Kunyange zvazvo marudzi akasiyana-siyana emagetsi eglucose anoshandisa physicochemical discovery akave akashumwa, kuderera kwekunzwa uye nguva inononoka yekupindura inoramba iri zvipingamupinyi kune inoenderera mberi glucose monitoring systems6,7,8.Mukuwedzera, ikozvino yakakurumbira electrochemical glucose sensors yakavakirwa pane enzymatic reactions ichiri nezvimwe zvisingakwanisi kunyangwe zvakanakira kupindura nekukurumidza, kunzwisiswa kwakanyanya uye nyore nyore kugadzira maitiro9,10.Nokudaro, marudzi akasiyana-siyana e-non-enzymatic electrochemical sensors ave akadzidzwa zvakanyanya kudzivirira enzyme denaturation apo achichengetedza zvakanakira electrochemical biosensors9,11,12,13.
Transition metal compounds (TMCs) vane basa rakakwana rinoita catalytic maererano neglucose, iyo inowedzera chiyero chekushandiswa kwavo mumagetsi emagetsi eglucose sensors13,14,15.Kusvika ikozvino, maitiro akasiyana-siyana anonzwisisika uye nzira dziri nyore dzekugadzirisa kweTMS dzakarongedzerwa kuti dziwedzere kunatsiridza kunzwisiswa, kusarudza, uye electrochemical kugadzikana kwekuonekwa kweglucose16,17,18.Semuyenzaniso, umbiguous transition metal oxides akadai mhangura oxide (CuO)11,19, zinc oxide (ZnO)20, nickel oxide (NiO)21,22, cobalt oxide (Co3O4)23,24 uye cerium oxide (CeO2) 25 ndiyo electrochemically inoshanda maererano neglucose.Kufambira mberi munguva pfupi yapfuura mubinary metal oxides se nickel cobaltate (NiCo2O4) yekuonekwa kweglucose yakaratidza mamwe maitiro ekubatanidza maererano nekuwedzera kwekuita kwemagetsi26,27,28,29,30.Kunyanya, kunyatsogadzirisa kuumbwa uye morphology kutonga kuumba TMS ine nanostructures yakasiyana-siyana inogona kuwedzera kuwedzera kunzwisiswa kwekuona nekuda kwenzvimbo yavo yakakura, saka inokurudzirwa zvikuru kukudziridza morphology inotungamirirwa TMS yekuvandudzwa kweglucose kuonekwa20,25,30,31,32, 33.34, 35.
Pano tinoshuma NiCo2O4 (NCO) nanomaterials ine akasiyana morphologies yekuonekwa kweglucose.NCO nanomaterials inowanikwa nenzira yakapfava hydrothermal uchishandisa zvakasiyana-siyana zvinowedzera, makemikari anowedzera chimwe chezvinhu zvakakosha mukuzvibatanidza kwenanostructures dzakasiyana-siyana morphologies.Isu takaongorora zvine hungwaru maitiro eNCO ane akasiyana morphologies pakuita kwavo kwe electrochemical yekuona glucose, kusanganisira kunzwa, kusarudza, kuderera kwekuona muganho, uye kugadzikana kwenguva refu.
Isu takagadzira NCO nanomaterials (yakapfupikiswa UNCO, PNCO, TNCO uye FNCO zvichiteerana) ine microstructures yakafanana neyegungwa urchins, pine tsono, tremella uye maruva.Mufananidzo 1 unoratidza akasiyana morphologies eUNCO, PNCO, TNCO, uye FNCO.Mifananidzo yeSEM ​​nemifananidzo yeEDS yakaratidza kuti Ni, Co, uye O zvakagoverwa zvakaenzana muNCO nanomaterials, sezvakaratidzwa muFigure 1 uye 2. S1 uye S2, zvichiteerana.Pamusoro pemuonde.2a,b inoratidza anomiririra TEM mifananidzo yeNCO nanomaterials ine morphology yakasiyana.UNCO i-self-assembling microsphere (diameter: ~ 5 µm) inoumbwa ne nanowires neNCO nanoparticles (avhareji yekukura kwechikamu: 20 nm).Iyi yakasarudzika microstructure inotarisirwa kupa nzvimbo yakakura yepasi kuti ifambise kupararira kwe electrolyte uye kutakura kweelectronic.Kuwedzerwa kweNH4F uye urea panguva yekubatanidza kwakakonzera kukora acicular microstructure (PNCO) 3 µm kureba uye 60 nm yakafara, inoumbwa nemanoparticles makuru.Kuwedzerwa kweHMT pachinzvimbo cheNH4F kunoguma mune tremello-senge morphology (TNCO) ine nanosheets akaunyana.Kuunzwa kweNH4F neHMT panguva yekubatanidza kunotungamira mukuunganidzwa kwepedyo akaunyana nanosheets, zvichikonzera maruva-senge morphology (FNCO).Mufananidzo weHREM (Fig. 2c) unoratidza mabhendi ekugezera akasiyana ane interplanar spacings ye0.473, 0.278, 0.50, uye 0.237 nm, inoenderana ne(111), (220), (311), uye (222) NiCo2O4 ndege, s 27. .Nzvimbo yakasarudzwa electron diffraction pattern (SAED) yeNCO nanomaterials (inset kuFig. 2b) yakasimbisawo polycrystalline nature yeNiCo2O4.Migumisiro ye-high-angle annular dark imaging (HAADF) uye EDS mapping inoratidza kuti zvinhu zvose zvakagoverwa zvakafanana muNCO nanomaterial, sezvakaratidzwa muFig. 2d.
Schematic mufananidzo wemaitiro ekuumbwa kweNiCo2O4 nanostructures ine controlled morphology.Schematics uye SEM mifananidzo yeakasiyana nanostructures inoratidzwa zvakare.
Morphological and structural characterization yeNCO nanomaterials: (a) TEM mufananidzo, (b) TEM mufananidzo pamwe neSAED patani, (c) grating-yakagadziriswa HRTEM mufananidzo uye inoenderana HADDF mifananidzo yeNi, Co, uye O mu (d) NCO nanomaterials..
X-ray diffraction maitiro eNCO nanomaterials emhando dzakasiyana siyana anoratidzwa muFig.3a.Iyo diffraction inokwira pa18.9, 31.1, 36.6, 44.6, 59.1 uye 64.9 ° inoratidza ndege (111), (220), (311), (400), (511) uye (440) NiCo2O4, zvichiteerana, idzo dzine cubic. spinel structure (JCPDS No. 20-0781) 36. Iyo FT-IR spectra yeNCO nanomaterials inoratidzwa muFig.3b.Mabhendi maviri akasimba ekudengenyeka munharaunda pakati pe555 ne669 cm-1 anoenderana nesimbi (Ni uye Co) okisijeni inotorwa kubva kune tetrahedral uye octahedral nzvimbo dzeNiCo2O437 spinel, zvichiteerana.Kuti unzwisise zviri nani maitiro eNCO nanomaterials, Raman spectra yakawanikwa sezvakaratidzwa muFig. 3c.Iwo mana enhongonya akaonekwa pa180, 459, 503, uye 642 cm-1 anoenderana neRaman modes F2g, E2g, F2g, uye A1g yeNiCo2O4 spinel, zvichiteerana.Zviyero zveXPS zvakaitwa kuona mamiriro emakemikari epamusoro ezvinhu muNCO nanomaterials.Pamusoro pemuonde.3d inoratidza XPS spectrum yeUNCO.Iyo spectrum yeNi 2p ine mahombe maviri epamusoro anowanikwa pakusunga masimba e854.8 uye 872.3 eV, anoenderana neNi 2p3/2 uye Ni 2p1/2, uye maviri evibrational satellite pa860.6 uye 879.1 eV, zvichiteerana.Izvi zvinoratidza kuvepo kweNi2+ uye Ni3+ oxidation nyika muNCO.Nzvimbo dzepamusoro dzakatenderedza 855.9 uye 873.4 eV ndedzeNi3+, uye dzepamusoro dzakatenderedza 854.2 ne871.6 eV ndedzeNi2+.Saizvozvo, iyo Co2p spectrum yemaviri spin-orbit doublets inoratidza hunhu hwepamusoro hweCo2+ uye Co3+ pa780.4 (Co 2p3/2) uye 795.7 eV (Co 2p1/2).Peaks pa796.0 uye 780.3 eV inoenderana neCo2+, uye inokwira pa794.4 uye 779.3 eV inoenderana neCo3+.Zvinofanira kucherechedzwa kuti polyvalent mamiriro esimbi ions (Ni2 +/ Ni3 + uye Co2 +/ Co3 +) muNiCo2O4 inokurudzira kuwedzera electrochemical basa37,38.Iyo Ni2p uye Co2p spectra yeUNCO, PNCO, TNCO, uye FNCO yakaratidza mhedzisiro yakafanana, sezvakaratidzwa mufig.S3.Mukuwedzera, iyo O1s spectra yeNCO nanomaterials yose (Fig. S4) yakaratidza zvikwiriso zviviri pa592.4 uye 531.2 eV, iyo yaibatanidza neyakajairwa simbi-okisijeni uye okisijeni zvisungo mumapoka ehydroxyl eNCO pamusoro, zvichiteerana39.Kunyangwe zvimiro zveNCO nanomaterials zvakafanana, misiyano yemorphological mune zvekuwedzera inoratidza kuti chimwe nechimwe chekuwedzera chinogona kutora chikamu zvakasiyana mukuita kwemakemikari kuumba NCO.Izvi zvinodzora iyo inesimba yakanaka yakanaka nucleation uye zviyo nhanho dzekukura, nekudaro kudzora particle size uye dhigirii reagglomeration.Nekudaro, kutonga kweakasiyana maitiro ma paramita, anosanganisira anowedzera, nguva yekuita, uye tembiricha panguva yekubatanidza, inogona kushandiswa kugadzira iyo microstructure uye kugadzirisa electrochemical kuita kweNCO nanomaterials yekuonekwa kweglucose.
(a) X-ray diffraction mapatani, (b) FTIR uye (c) Raman spectra yeNCO nanomaterials, (d) XPS spectra yeNi 2p uye Co 2p kubva kuUNCO.
Iyo morphology yeiyo yakagadziridzwa NCO nanomaterials yakanyatso hukama nekuumbwa kwezvikamu zvekutanga zvakawanikwa kubva kune akasiyana ekuwedzera anoratidzwa muFigure S5.Mukuwedzera, X-ray uye Raman spectra yemasampuli achangobva kugadzirirwa (Figus S6 uye S7a) yakaratidza kuti kubatanidzwa kwezvimwe zvakasiyana-siyana zvemakemikari zvakakonzera kusiyana kwecrystallographic: Ni uye Co carbonate hydroxides yainyanya kuonekwa mumakungwa egungwa uye pine tsono chimiro, apo se zvimiro muchimiro che tremella uye ruva zvinoratidza kuvapo nickel uye cobalt hydroxides.Iyo FT-IR uye XPS spectra yemasampuri akagadzirirwa anoratidzwa muMifananidzo 1 uye 2. S7b-S9 inopawo uchapupu hwakajeka hwekusiyana kwekristallographic yambotaurwa.Kubva pane zvigadzirwa zvemasampuli akagadzirirwa, zvinova pachena kuti zvinowedzera zvinobatanidzwa mukuita kwehydrothermal uye zvinopa nzira dzakasiyana dzekuita kuti uwane zvikamu zvekutanga nemamorphologies akasiyana40,41,42.Kuzvibatanidza kwema morphologies akasiyana, anosanganisira one-dimensional (1D) nanowires uye maviri-dimensional (2D) nanosheets, anotsanangurwa neakasiyana kemikari mamiriro ekutanga kwezvikamu (Ni uye Co ions, pamwe nemapoka anoshanda), inoteverwa nekristal growth42, 43, 44, 45, 46, 47. Munguva ye-post-thermal processing, zvikamu zvakasiyana-siyana zvekutanga zvinoshandurwa kuva NCO spinel pavanenge vachichengetedza morphology yavo yakasiyana, sezvakaratidzwa muFigure 1 uye 2. 2 uye 3a.
Morphological misiyano muNCO nanomaterials inogona kukanganisa iyo electrochemically inoshanda pamusoro nzvimbo yekuona glucose, nekudaro ichitarisa iyo yakazara electrochemical maitiro eiyo glucose sensor.Iyo N2 BET adsorption-desorption isotherm yakashandiswa kufungidzira saizi yepore uye chaiyo nzvimbo yeNCO nanomaterials.Pamusoro pemuonde.4 inoratidza BET isotherms yeakasiyana NCO nanomaterials.Iyo BET chaiyo nzvimbo yeUNCO, PNCO, TNCO uye FNCO yakafungidzirwa pa45.303, 43.304, 38.861 uye 27.260 m2 / g, zvichiteerana.UNCO ine yepamusoro-soro BET pamusoro nzvimbo (45.303 m2 g-1) uye hombe pore vhoriyamu (0.2849 cm3 g-1), uye pore saizi kuparadzirwa kwakamanikana.Migumisiro yeBET yeNCO nanomaterials inoratidzwa muTebhu 1. N2 adsorption-desorption curves yakanga yakafanana zvikuru nemhando IV isothermal hysteresis loops, zvichiratidza kuti sampuli dzose dzine mesoporous structure48.Mesoporous UNCOs ine nzvimbo yepamusoro yepamusoro uye yepamusoro pore vhoriyamu inotarisirwa kupa akawanda anoshanda masaiti ezvekuita redox, zvichitungamira mukuvandudzwa kwekuita kwe electrochemical.
BET zvawanikwa zve (a) UNCO, (b) PNCO, (c) TNCO, uye (d) FNCO.Iyo inset inoratidza inoenderana pore saizi yekugovera.
Iyo electrochemical redox maitiro eNCO nanomaterials ane akasiyana morphologies ekuonekwa kweglucose akaongororwa pachishandiswa CV kuyerwa.Pamusoro pemuonde.5 inoratidza CV macurves eNCO nanomaterials mu 0.1 M NaOH alkaline electrolyte ine uye isina 5 mM glucose pachiyero che 50 mVs-1.Mukusavapo kweglucose, mapeji eredox akaonekwa pa 0.50 uye 0.35 V, inoenderana neoxidation yakabatana neM-O (M: Ni2 +, Co2 +) uye M * -O-OH (M *: Ni3 +, Co3 +).kushandisa OH anion.Mushure mekuwedzera kwe5 mM glucose, redox reaction pamusoro peNCO nanomaterials yakawedzera zvakanyanya, izvo zvingave zvakakonzerwa neoxidation yeglucose kune gluconolactone.Mufananidzo S10 inoratidza peak redox currents pa scan rate ye 5–100 mV s-1 mu 0.1 M NaOH mhinduro.Zviri pachena kuti peak redox ikozvino inowedzera nekuwedzera scan rate, zvichiratidza kuti NCO nanomaterials ine yakafanana diffusion controlled electrochemical behaviour50,51.Sezvinoratidzwa mumufananidzo S11, iyo electrochemical surface area (ECSA) yeUNCO, PNCO, TNCO, uye FNCO inofungidzirwa kuva 2.15, 1.47, 1.2, uye 1.03 cm2, maererano.Izvi zvinoratidza kuti UNCO inobatsira kune electrocatalytic process, kufambisa kuonekwa kweglucose.
CV macurves e (a) UNCO, (b) PNCO, (c) TNCO, uye (d) FNCO maelectrodes asina glucose uye anowedzerwa ne5 mM glucose pachiyero che50 mVs-1.
Iyo electrochemical performance yeNCO nanomaterials yekuonekwa kweglucose yakaongororwa uye mhedzisiro inoratidzwa muFig. 6. Glucose senitivity yakagadziriswa neCA nzira kuburikidza nekuwedzera zvishoma nezvishoma zvakasiyana-siyana zveglucose (0.01-6 mM) mu 0.1 M NaOH solution pa 0.5 V ine nguva ye60 s.Sezvinoratidzwa mufig.6a–d, NCO nanomaterials inoratidza kunzwisiswa kwakasiyana kubva pa84.72 kusvika 116.33 µA mM-1 cm-2 ine high coefficients yekubatanidza (R2) kubva pa0.99 kusvika 0.993.Iyo calibration curve pakati peglucose concentration uye kuita kwazvino kweNCO nanomaterials inoratidzwa mufig.S12.Iyo yakaverengerwa miganho yekuonekwa (LOD) yeNCO nanomaterials yaive muhuwandu hwe0.0623–0.0783 µM.Zvinoenderana nemhedzisiro yeCA bvunzo, UNCO yakaratidza kunzwisiswa kwakanyanya (116.33 μA mM-1 cm-2) munzvimbo yakakura yekuona.Izvi zvinogona kutsanangurwa neiyo yakasarudzika yegungwa urchin-senge morphology, ine mesoporous chimiro chine hombe chaiyo nzvimbo inopa akawanda anoshanda nzvimbo dzeglucose marudzi.Kuita kwe electrochemical kweNCO nanomaterials yakaratidzwa muTable S1 inosimbisa kunaka kwe electrochemical glucose yekuona kuita kweNCO nanomaterials yakagadzirirwa muchidzidzo ichi.
CA mhinduro dzeUNCO (a), PNCO (b), TNCO (c), neFNCO (d) maelectrodes ane glucose yakawedzerwa ku 0.1 M NaOH solution pa 0.50 V. The insets inoratidza calibration curves of current responses dzeNCO nanomaterials: (e ) KA mhinduro dzeUNCO, (f) PNCO, (g) TNCO, uye (h) FNCO nekuwedzera zvishoma nezvishoma kwe1 mM glucose uye 0.1 mM zvinokanganisa zvinhu (LA, DA, AA, uye UA).
Kugona kunopesana nekupindira kwekuonekwa kweglucose ndechimwe chinhu chinokosha pakusarudzwa uye kunzwisisika kweglucose nekuvhiringidza makemikari.Pamusoro pemuonde.6e–h inoratidza kugona kupindira kweNCO nanomaterials mu 0.1 M NaOH mhinduro.Mamorekuru anopindira akadai se LA, DA, AA uye UA anosarudzwa uye anowedzerwa kune electrolyte.Mhinduro yazvino yeNCO nanomaterials kune glucose inooneka.Zvakadaro, mhinduro yazvino kuUA, DA, AA neLA haina kushanduka, zvinoreva kuti maNCO nanomaterials airatidza kusarudzika kwakanaka kwekuonekwa kweglucose zvisinei nekusiyana kwavo kwemorphological.Mufananidzo S13 unoratidza kugadzikana kweNCO nanomaterials yakaongororwa neCA mhinduro mu 0.1 M NaOH, apo 1 mM glucose yakawedzerwa ku electrolyte kwenguva yakareba (80,000 s).Ikozvino mhinduro dzeUNCO, PNCO, TNCO, uye FNCO dzaive 98.6%, 97.5%, 98.4%, uye 96.8%, maererano, yepakutanga ikozvino nekuwedzera kwekuwedzera 1 mM glucose mushure me80,000 s.Yese NCO nanomaterials inoratidza yakagadzikana redox maitiro nemhando yeglucose kwenguva yakareba.Kunyanya, iyo UNCO yemazuva ano chiratidzo haina kungochengeta 97.1% yekutanga ikozvino, asiwo yakachengetedza morphology yayo uye chemikemikari bond properties mushure memazuva manomwe ezvakatipoteredza kwenguva refu kugadzikana kwekuedza (Figus S14 uye S15a).Mukuwedzera, kubereka uye kubereka kweUNCO kwakaedzwa sezvinoratidzwa muFig. S15b, c.Iyo yakaverengerwa Relative Standard Deviation (RSD) yekuberekana uye kudzokorora yaive 2.42% uye 2.14%, zvichiteerana, zvichiratidza zvingangoita mashandisirwo seyeindasitiri giredhi glucose sensor.Izvi zvinoratidza kugadzikana kwakanaka uye kugadzikana kwemakemikari kweUNCO pasi peoxidizing mamiriro ekuonekwa kweglucose.
Zviri pachena kuti electrochemical performance yeNCO nanomaterials yekuona glucose inonyanya kuenderana nemaitiro ekugadzirisa kwechikamu chekutanga chakagadzirirwa ne hydrothermal nzira ine additives (Fig. S16).Nzvimbo yepamusoro yeUNCO ine nzvimbo dzakawanda dzemagetsi kupfuura mamwe nanostructures, iyo inobatsira kuvandudza redox reaction pakati pezvinhu zvinoshanda uye glucose particles.Iyo mesoporous chimiro cheUNCO inogona kufumura zviri nyore mamwe maNi uye Co masaiti kune electrolyte kuona glucose, zvichikonzera kukurumidza kwe electrochemical mhinduro.Imwe-dimensional nanowires muUNCO inogona kuwedzera chiyero chekupararira nekupa mapfupi nzira dzekufambisa dzeiyoni nemaerekitironi.Nekuda kweiyo yakasarudzika maumbirwo ataurwa pamusoro, kuita kwe electrochemical yeUNCO yekuona glucose yakakura kupfuura iyo yePNCO, TNCO, uye FNCO.Izvi zvinoratidza kuti iyo yakasarudzika UNCO morphology ine nzvimbo yepamusoro yepamusoro uye saizi yepore inogona kupa yakanakisa electrochemical kuita kwekuonekwa kweglucose.
Mhedzisiro yenzvimbo chaiyo yenzvimbo pane electrochemical maitiro eNCO nanomaterials yakadzidzwa.NCO nanomaterials ine nzvimbo yakasiyana yakasarudzika yakawanikwa nenzira yakapusa yehydrothermal uye akasiyana ekuwedzera.Zvimwe zvinowedzera panguva yekubatanidza zvinopinda mune zvakasiyana-siyana zvemakemikari maitiro uye zvinogadzira zvikamu zvakasiyana zvekutanga.Izvi zvakakonzera kuzvibatanidza kwakasiyana-siyana nanostructures ine morphologies yakafanana nehedgehog, pine tsono, tremella, uye ruva.Kutevera mushure mekupisa kunotungamira kune yakafanana kemikari mamiriro ekristaro NCO nanomaterials ine spinel chimiro ichichengetedza yavo yakasarudzika morphology.Zvichienderana nenzvimbo yezvakasiyana morphology, iyo electrochemical performance yeNCO nanomaterials yekuonekwa kweglucose yakagadziridzwa zvakanyanya.Kunyanya, kunzwisiswa kweglucose yeNCO nanomaterials ine sea urchin morphology yakawedzera kusvika 116.33 µA mM-1 cm-2 ine high coefficient (R2) ye0.99 mumutsara we 0.01-6 mM.Iri basa rinogona kupa hwaro hwesainzi hweinjiniya yemorphological kugadzirisa chaiyo nzvimbo uye kuwedzera kuvandudza kushanda kwe electrochemical yeasiri-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) uye uric acid (UA) yakatengwa kubva kuSigma-Aldrich.Mareagents ese akashandiswa aive egiredhi rekuongorora uye akashandiswa pasina kumwe kucheneswa.
NiCo2O4 yakagadzirwa nenzira yakapfava yehydrothermal inoteverwa nekurapa kwekupisa.Muchidimbu: 1 mmol ye nickel nitrate (Ni(NO3) 2∙6H2O) uye 2 mmol yecobalt nitrate (Co(NO3)2∙6H2O) yakanyungudutswa mu30 ml yemvura yakasvibiswa.Kuti udzore morphology yeNiCo2O4, zvinowedzerwa senge urea, ammonium fluoride uye hexamethylenetetramine (HMT) zvakasarudzwa zvakawedzerwa kune mhinduro iri pamusoro.Musanganiswa wose wakabva waendeswa kune 50 ml Teflon-lined autoclave uye yakagadziriswa nehydrothermal reaction muvheni ye convection pa 120 ° C. kwemaawa matanhatu.Mushure mekutonhodzwa kwechisikigo kusvika kune tembiricha yekamuri, iyo inokonzeresa mvura yakagezwa uye yakagezwa kakawanda nemvura yakasvibiswa uye ethanol, ndokuzoomeswa husiku hwese pa60 ° C.Mushure maizvozvi, masampuli matsva akagadzirirwa akacheneswa pa400 ° C kwe4 h mumhepo yakadzikama.Ruzivo rwezviedzo rwakanyorwa muSupplementary Information Table S2.
X-ray diffraction analysis (XRD, X'Pert-Pro MPD; PANalytical) yakaitwa pachishandiswa Cu-Kα mwaranzi (λ = 0.15418 nm) pa40 kV uye 30 mA kuti idzidze maitiro ezvimiro zveNCO nanomaterials yose.Diffraction maitiro akarekodhwa muhuwandu hwemakona 2θ 10-80 ° ine nhanho ye0.05 °.Surface morphology uye microstructure zvakaongororwa pachishandiswa munda emission scanning electron microscopy (FESEM; Nova SEM 200, FEI) uye scanning transmission electron microscopy (STEM; TALOS F200X, FEI) ine simba dispersive X-ray spectroscopy (EDS).Iyo valence inoti yepasi yakaongororwa neX-ray photoelectron spectroscopy (XPS; PHI 5000 Versa Probe II, ULVAC PHI) vachishandisa Al Kα radiation (hν = 1486.6 eV).Simba rinosunga rakagadziriswa uchishandisa C 1 s peak pa 284.6 eV sereferensi.Mushure mekugadzira sampuli pa KBr particles, Fourier kushandura infrared (FT-IR) spectra yakanyorwa muwavenumber range 1500–400 cm–1 paJasco-FTIR-6300 spectrometer.Raman spectra yakawanikwa zvakare pachishandiswa Raman spectrometer (Horiba Co., Japan) ine He-Ne laser (632.8 nm) senzvimbo yekunakidzwa.Brunauer-Emmett-Teller (BET; BELSORP mini II, MicrotracBEL, Corp.) akashandisa BELSORP mini II analyzer (MicrotracBEL Corp.) kuyera tembiricha yakaderera N2 adsorption-desorption isotherms kuti ifungidzire nzvimbo chaiyo uye kugoverwa kwepore saizi.
Zvose zviyero zve electrochemical, zvakadai se cyclic voltammetry (CV) uye chronoamperometry (CA), yakaitwa paPGSTAT302N potentiostat (Metrohm-Autolab) pakupisa kwekamuri uchishandisa matatu-electrode system mu 0.1 M NaOH aqueous solution.Electrode inoshanda yakavakirwa pagirazi kabhoni electrode (GC), Ag/AgCl electrode, uye platinum ndiro yakashandiswa seye electrode inoshanda, referensi electrode, uye counter electrode, zvichiteerana.MaCV akanyorwa pakati pe0 ne0.6 V pamitengo yakasiyana-siyana ye5-100 mV s-1.Kuyera ECSA, CV yakaitwa muhuwandu hwe 0.1-0.2 V pamhando dzakasiyana dze scan (5-100 mV s-1).Tora sampuli yeCA reaction yeglucose pa 0.5 V nekukurudzira.Kuyera kunzwa uye kusarudza, shandisa 0.01–6 mM glucose, 0.1 mM LA, DA, AA, uye UA mu 0.1 M NaOH.Kuberekwazve kweUNCO kwakaedzwa uchishandisa ma electrode matatu akasiyana akawedzerwa ne5 mM glucose pasi pemamiriro akanaka.Iko kudzokororwa kwakaongororwawo nekuita zviyero zvitatu neUNCO electrode mukati maawa matanhatu.
Yese data yakagadzirwa kana kuongororwa muchidzidzo ichi inosanganisirwa mune ino chinyorwa chakabudiswa (uye faira rayo rekuwedzera ruzivo).
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