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TiO2 ndi chinthu chopangidwa ndi semiconductor chomwe chimagwiritsidwa ntchito posintha magetsi kukhala kuwala. Pofuna kupititsa patsogolo kugwiritsa ntchito kuwala, tinthu tating'onoting'ono ta nickel ndi siliva sulfide tinapangidwa pamwamba pa ma nanowaya a TiO2 pogwiritsa ntchito njira yosavuta yoviika ndi kutsitsa kuwala. Kafukufuku wotsatira wa momwe Ag/NiS/TiO2 nanocomposites amatetezera magetsi pogwiritsa ntchito chitsulo chosapanga dzimbiri cha 304 wachitika, ndipo mawonekedwe, kapangidwe, ndi mawonekedwe a kuyamwa kwa kuwala kwa zinthuzo zawonjezeredwa. Zotsatira zake zikusonyeza kuti ma nanocomposites a Ag/NiS/TiO2 okonzedwa amatha kupereka chitetezo chabwino kwambiri cha cathodic cha chitsulo chosapanga dzimbiri cha 304 pamene kuchuluka kwa nickel sulfide impregnation-precipitation cycles kuli 6 ndipo kuchuluka kwa siliva nitrate photoreduction kuli 0.1M.
Kugwiritsa ntchito ma semiconductor a mtundu wa n poteteza photocathode pogwiritsa ntchito kuwala kwa dzuwa kwakhala nkhani yofunika kwambiri m'zaka zaposachedwa. Akakhudzidwa ndi kuwala kwa dzuwa, ma elekitironi ochokera ku valence band (VB) a semiconductor ma elekitironi amalowetsedwa mu conduction band (CB) kuti apange ma elekitironi opangidwa ndi photo. Ngati conduction band potential ya semiconductor kapena nanocomposite ili ndi negative kuposa self-etching potential ya bound metal, ma elekitironi opangidwa ndi photo awa amasamutsira pamwamba pa bound metal. Kusonkhanitsa ma elekitironi kudzatsogolera ku cathodic polarization ya chitsulo ndikupereka cathodic protection ya cathodic metal 1,2,3,4,5,6,7. Semiconductor material amaonedwa kuti ndi photoanode yosapereka nsembe, popeza anodic reaction siiwononga semiconductor material yokha, koma oxidation ya madzi kudzera m'mabowo opangidwa ndi photo kapena adsorbed organic pollutions, kapena kukhalapo kwa osonkhanitsa kuti agwire mabowo opangidwa ndi photo. Chofunika kwambiri, semiconductor material ayenera kukhala ndi CB potential yomwe ili negative kuposa corrosion potential ya chitsulo chomwe chikutetezedwa. Pokhapokha ma elekitironi opangidwa ndi photogeneration amatha kuchoka pa conduction band ya semiconductor kupita ku chitsulo chotetezedwa. Kafukufuku wokhudzana ndi kukana dzimbiri pogwiritsa ntchito photochemical wayang'ana kwambiri pa zinthu zopangidwa ndi semiconductor za inorganic n-type zomwe zili ndi mipata yayikulu (3.0–3.2EV)1,2,3,4,5,6,7, zomwe zimangoyankha kuwala kwa ultraviolet (<400 nm), zomwe zimachepetsa kupezeka kwa kuwala. Kafukufuku wokhudzana ndi kukana dzimbiri pogwiritsa ntchito photochemical wayang'ana kwambiri pa zinthu zopangidwa ndi semiconductor za inorganic n-type zomwe zili ndi mipata yayikulu (3.0–3.2EV)1,2,3,4,5,6,7, zomwe zimangoyankha kuwala kwa ultraviolet (<400 nm), zomwe zimachepetsa kupezeka kwa kuwala. Исследования стойкости к фотохимической коррозии были сосредоточены на неорганических полупроводниковых материалах n-типа с широзеной,3,3 EV)1,2,3,4,5,6,7, которые реагируют только на ультрафиолетовое излучение (< 400 нм), уменьшение доступности света. Kafukufuku wokhudza kukana kwa dzimbiri pogwiritsa ntchito photochemical wayang'ana kwambiri pa zinthu za semiconductor za mtundu wa n zomwe zili ndi bandgap yayikulu (3.0–3.2 EV)1,2,3,4,5,6,7 zomwe zimangoyankha ku kuwala kwa ultraviolet (<400 nm), kuchepa kwa kupezeka kwa kuwala.光化学耐腐蚀性研究主要集中在具有宽带隙(3.0–3.2EV)1,2,3,4,5,6,7 的无机n型半导体材料上，這些材料仅对紫外光（< 400 nm）有响应，减少光的可用性.光 化学 耐腐 蚀性 研究 主要 在 具有 宽带隙 宽带隙 宽带隙 (3.0–3.2ev) 1.2,3,4,7, 6,材料 上， 這些 材料 仅 对 (<400 nm) 有 有 有 有 有 有 有 有 有 有 有 有 有响应，减少光的可用性. Исследования стойкости к фотохимической коррозии в основном были сосредоточены на неорганических полупроводниковых материалах пизешен (3,0–3,2EV)1,2,3,4,5,6,7, которые чувствительны только к УФ-излучению (<400 нм). Kafukufuku wokhudza kukana dzimbiri pogwiritsa ntchito photochemical wayang'ana kwambiri pa zinthu za semiconductor za mtundu wa inorganic zomwe sizimakhudzidwa ndi kuwala kwa UV kokha (<400 nm).Poyankha, kupezeka kwa kuwala kumachepa.
Pankhani yoteteza dzimbiri la m'nyanja, ukadaulo woteteza cathodic wa photoelectrochemical umagwira ntchito yofunika kwambiri. TiO2 ndi chinthu cha semiconductor chomwe chimayamwa bwino kwambiri kuwala kwa UV komanso mphamvu zowunikira kuwala. Komabe, chifukwa cha kuchuluka kochepa kwa kuwala, mabowo a ma elekitironi opangidwa ndi photoelectrochemical amalumikizananso mosavuta ndipo sangatetezedwe mumdima. Kafukufuku wowonjezereka akufunika kuti apeze yankho loyenera komanso lotheka. Zanenedwa kuti njira zambiri zosinthira pamwamba zingagwiritsidwe ntchito kupititsa patsogolo kuwala kwa TiO2, monga kugwiritsa ntchito mankhwala osokoneza bongo ndi Fe, N, ndikusakaniza ndi Ni3S2, Bi2Se3, CdTe, ndi zina zotero. Chifukwa chake, TiO2 composite yokhala ndi zinthu zomwe zimakhala ndi mphamvu zambiri zosinthira kuwala imagwiritsidwa ntchito kwambiri pachitetezo cha cathodic chopangidwa ndi photoelectrochemical.
Nickel sulfide ndi chinthu cha semiconductor chokhala ndi mpata wopapatiza wa band wa 1.24 eV8.9 yokha. Mpata wopapatiza ukachepa, kugwiritsa ntchito kuwala kumakhala kolimba. Nickel sulfide ikasakanizidwa ndi pamwamba pa titanium dioxide, kuchuluka kwa kugwiritsa ntchito kuwala kumatha kuwonjezeka. Kuphatikiza ndi titanium dioxide, kumatha kukonza bwino magwiridwe antchito a ma elekitironi ndi mabowo opangidwa ndi photocatalytic. Nickel sulfide imagwiritsidwa ntchito kwambiri popanga hydrogen yamagetsi, mabatire ndi kuwonongeka kwa zinthu zodetsa8,9,10. Komabe, kugwiritsidwa ntchito kwake poteteza photocathode sikunanenedwebe. Mu kafukufukuyu, chida chopapatiza cha bandgap semiconductor chidasankhidwa kuti chithetse vuto la kugwiritsa ntchito bwino kuwala kwa TiO2. Tinthu tating'onoting'ono ta nickel ndi siliva sulfide tinamangiriridwa pamwamba pa ma nanowaya a TiO2 mwa kumiza ndi njira zochepetsera kuwala, motsatana. Nanocomposite ya Ag/NiS/TiO2 imawongolera magwiridwe antchito a kuwala ndikukulitsa kuchuluka kwa kuyamwa kwa kuwala kuchokera kudera la ultraviolet kupita kudera looneka. Pakadali pano, kuyika kwa tinthu tating'onoting'ono ta siliva kumapatsa Ag/NiS/TiO2 nanocomposite kukhazikika bwino kwa kuwala komanso chitetezo chokhazikika cha cathodic.
Choyamba, pepala la titaniyamu lokhala ndi makulidwe a 0.1 mm lokhala ndi chiyero cha 99.9% linadulidwa kufika pa kukula kwa 30 mm × 10 mm poyesera. Kenako, pamwamba pa pepala lililonse la titaniyamu linapukutidwa ka 100 ndi sandpaper ya grit 2500, kenako n’kutsukidwa motsatizana ndi acetone, ethanol yokwanira, ndi madzi osungunuka. Ikani mbale ya titaniyamu mu chisakanizo cha 85 °C (sodium hydroxide: sodium carbonate: madzi = 5:2:100) kwa mphindi 90, chotsani ndikutsuka ndi madzi osungunuka. Pamwamba pake panadulidwa ndi yankho la HF (HF:H2O = 1:5) kwa mphindi imodzi, kenako n’kutsukidwa mosinthana ndi acetone, ethanol, ndi madzi osungunuka, kenako n’kuumitsa kuti mugwiritse ntchito. Mawaya a titaniyamu dioxide nanowaya anapangidwa mofulumira pamwamba pa pepala la titaniyamu pogwiritsa ntchito njira imodzi yosungunuka. Pa anodizing, njira yachikhalidwe ya ma electrode awiri imagwiritsidwa ntchito, electrode yogwira ntchito ndi pepala la titaniyamu, ndipo counter electrode ndi platinum electrode. Ikani mbale ya titaniyamu mu 400 ml ya yankho la 2 M NaOH pogwiritsa ntchito ma electrode clamps. Mphamvu yamagetsi ya DC imakhala yokhazikika pa 1.3 A. Kutentha kwa yankho kunasungidwa pa 80°C kwa mphindi 180 panthawi ya systemic reaction. Pepala la titaniyamu linachotsedwa, kutsukidwa ndi acetone ndi ethanol, kutsukidwa ndi madzi osungunuka, ndikuumitsidwa mwachilengedwe. Kenako zitsanzozo zinayikidwa mu uvuni wa muffle pa 450°C (kutentha kwa 5°C/min), kusungidwa kutentha kosasintha kwa mphindi 120, ndikuyikidwa mu thireyi yowumitsira.
Chosakaniza cha nickel sulfide-titanium dioxide chinapezeka mwa njira yosavuta komanso yosavuta yoyeretsera. Choyamba, nickel nitrate (0.03 M) inasungunuka mu ethanol ndikusungidwa pansi pa kusakaniza kwa maginito kwa mphindi 20 kuti mupeze yankho la ethanol la nickel nitrate. Kenako konzani sodium sulfide (0.03 M) ndi yankho losakanikirana la methanol (methanol:madzi = 1:1). Kenako, mapiritsi a titanium dioxide anayikidwa mu yankho lomwe linakonzedwa pamwambapa, kuchotsedwa patatha mphindi 4, ndikutsukidwa mwachangu ndi yankho losakanikirana la methanol ndi madzi (methanol:madzi = 1:1) kwa mphindi 1. Pambuyo poti pamwamba pauma, mapiritsiwo anayikidwa mu uvuni wosungunuka, kutenthedwa mu vacuum pa 380°C kwa mphindi 20, kuziziritsidwa kutentha kwa chipinda, ndikuwuma. Chiwerengero cha maulendo 2, 4, 6 ndi 8.
Ma nanoparticles a Ag adasinthidwa ma nanocomposites a Ag/NiS/TiO2 pogwiritsa ntchito photoreduction12,13. Nanocomposite ya Ag/NiS/TiO2 yomwe idapezeka idayikidwa mu yankho la siliva la nitrate lofunikira pakuyesera. Kenako zitsanzozo zidawotchedwa ndi kuwala kwa ultraviolet kwa mphindi 30, pamwamba pake padatsukidwa ndi madzi osasungunuka, ndipo ma nanocomposites a Ag/NiS/TiO2 adapezeka powumitsa mwachilengedwe. Njira yoyesera yomwe yafotokozedwa pamwambapa ikuwonetsedwa pa Chithunzi 1.
Ma nanocomposites a Ag/NiS/TiO2 amadziwika kwambiri ndi ma microscopy a electron scanning field emission (FESEM), energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), ndi diffuse reflectance mu ultraviolet ndi visible ranges (UV-Vis). FESEM idachitika pogwiritsa ntchito Nova NanoSEM 450 microscope (FEI Corporation, USA). Kufulumizitsa voltage 1 kV, spot size 2.0. Chipangizochi chimagwiritsa ntchito CBS probe kuti chilandire ma electron achiwiri ndi ambuyo kuti ayese topography. EMF idachitika pogwiritsa ntchito Oxford X-Max N50 EMF system (Oxford Instruments Technology Co., Ltd.) yokhala ndi voltage yothamanga ya 15 kV ndi spot size ya 3.0. Kusanthula kwabwino komanso kochuluka pogwiritsa ntchito ma X-ray odziwika bwino. Kujambula kwa X-ray photoelectron spectroscopy kunachitika pa Escalab 250Xi spectrometer (Thermo Fisher Scientific Corporation, USA) yomwe imagwira ntchito munjira yokhazikika yamphamvu yokhala ndi mphamvu yosonkhezera ya 150 W ndi monochromatic Al Kα radiation (1486.6 eV) ngati gwero losonkhezera. Kujambula konse kwa 0–1600 eV, mphamvu yonse ya 50 eV, m'lifupi mwa sitepe ya 1.0 eV, ndi kaboni wosayera (~284.8 eV) zinagwiritsidwa ntchito ngati zizindikiro zowongolera mphamvu yomangira. Mphamvu yodutsa pakujambula kopapatiza inali 20 eV yokhala ndi sitepe ya 0.05 eV. Kujambula kwa Diffuse reflectance spectroscopy m'dera looneka ndi UV kunachitidwa pa Cary 5000 spectrometer (Varian, USA) yokhala ndi mbale yokhazikika ya barium sulfate mumtundu wa scanning wa 10–80°.
Mu ntchito iyi, kapangidwe kake (kulemera kwa peresenti) ka chitsulo chosapanga dzimbiri 304 ndi 0.08 C, 1.86 Mn, 0.72 Si, 0.035 P, 0.029 s, 18.25 Cr, 8.5 Ni, ndipo chotsalacho ndi Fe. 10mm x 10mm x 10mm 304 chitsulo chosapanga dzimbiri, epoxy yophimbidwa ndi malo owonekera a 1 cm2. Pamwamba pake panapakidwa mchenga ndi sandpaper ya silicon carbide ya 2400 grit ndikutsukidwa ndi ethanol. Chitsulo chosapanga dzimbiricho chinayikidwa mu madzi oyeretsedwa kwa mphindi 5 kenako nkusungidwa mu uvuni.
Mu kuyesera kwa OCP, zitsulo zosapanga dzimbiri 304 ndi photoanode ya Ag/NiS/TiO2 zinayikidwa mu selo yowononga ndi selo ya photoanode, motsatana (Chithunzi 2). Selo yowononga inadzazidwa ndi yankho la 3.5% NaCl, ndipo 0.25 M Na2SO3 inathiridwa mu selo ya photoanode ngati msampha wa dzenje. Ma electrolyte awiriwa analekanitsidwa ndi chisakanizocho pogwiritsa ntchito nembanemba ya naphthol. OCP inayesedwa pa malo ogwirira ntchito a electrochemical (P4000+, USA). Electrode yowunikira inali electrode ya calomel yokhuta (SCE). Gwero la kuwala (xenon lamp, PLS-SXE300C, Poisson Technologies Co., Ltd.) ndi mbale yodulidwa 420 zinayikidwa pamalo otulukira kuwala, zomwe zimathandiza kuti kuwala kowoneka kudutsa mugalasi la quartz kupita ku photoanode. Electrode ya 304 yachitsulo chosapanga dzimbiri imalumikizidwa ku photoanode ndi waya wamkuwa. Kuyesera kusanachitike, electrode ya 304 stainless steel inanyowa mu yankho la 3.5% NaCl kwa maola awiri kuti iwonetsetse kuti zinthu zikuyenda bwino. Poyamba kuyesaku, magetsi akayatsidwa ndi kuzimitsidwa, ma elekitironi othamanga a photoanode amafika pamwamba pa 304 stainless steel kudzera mu waya.
Mu zoyeserera pa kuchuluka kwa photocurrent, ma photoanode a 304SS ndi Ag/NiS/TiO2 adayikidwa m'maselo a dzimbiri ndi ma cell a photoanode, motsatana (Chithunzi 3). Kuchuluka kwa photocurrent kunayesedwa pa dongosolo lomwelo ndi OCP. Kuti mupeze kuchuluka kwenikweni kwa photocurrent pakati pa chitsulo chosapanga dzimbiri cha 304 ndi photoanode, potentiostat idagwiritsidwa ntchito ngati zero resistance ammeter kuti ilumikize chitsulo chosapanga dzimbiri cha 304 ndi photoanode pansi pa mikhalidwe yopanda polarized. Kuti tichite izi, ma reference ndi counter electrodes mu zoyeserera adafupikitsidwa, kotero kuti electrochemical workstation imagwira ntchito ngati zero-resistance ammeter yomwe imatha kuyeza kuchuluka kwenikweni kwa current. Electrode ya 304 stainless steel imalumikizidwa pansi pa electrochemical workstation, ndipo photoanode imalumikizidwa ndi electrode clamp yogwira ntchito. Poyamba zoyeserera, pamene kuwala kumayatsidwa ndikuzimitsidwa, ma electron othamanga a photoanode kudzera mu waya amafika pamwamba pa 304 stainless steel. Pa nthawiyi, kusintha kwa kuchuluka kwa photocurrent pamwamba pa chitsulo chosapanga dzimbiri cha 304 kungawonekere.
Kuti aphunzire momwe ma nanocomposites amagwirira ntchito pa chitsulo chosapanga dzimbiri cha 304, kusintha kwa mphamvu ya photoionization ya chitsulo chosapanga dzimbiri cha 304 ndi ma nanocomposites, komanso kusintha kwa kuchuluka kwa photoionization pakati pa ma nanocomposites ndi ma 304 osapanga dzimbiri, kunayesedwa.
Pa chithunzi 4 chikuwonetsa kusintha kwa mphamvu ya open circuit ya 304 stainless steel ndi nanocomposites pansi pa kuwala kowoneka bwino komanso pansi pa mdima. Pa chithunzi 4a chikuwonetsa mphamvu ya nthawi yoyika NiS poyimitsidwa pa mphamvu ya open circuit, ndipo chithunzi 4b chikuwonetsa momwe kuchuluka kwa nitrate ya siliva kumakhudzira mphamvu ya open circuit panthawi yochepetsa kuwala. Pa chithunzi 4a chikuwonetsa kuti mphamvu ya open circuit ya NiS/TiO2 nanocomposite yolumikizidwa ku 304 stainless steel imachepa kwambiri panthawi yomwe nyali imayatsidwa poyerekeza ndi nickel sulfide composite. Kuphatikiza apo, mphamvu ya open circuit ndi yoipa kwambiri kuposa ya ma nanowaya oyera a TiO2, zomwe zikusonyeza kuti nickel sulfide composite imapanga ma electron ambiri ndikuwongolera mphamvu ya photocathode yoteteza kuchokera ku TiO2. Komabe, pamapeto pake, mphamvu ya no-load imakwera mofulumira kufika pa mphamvu ya no-load ya chitsulo chosapanga dzimbiri, zomwe zikusonyeza kuti nickel sulfide ilibe mphamvu yosungira mphamvu. Zotsatira za kuchuluka kwa ma immersion deposition cycles pa open circuit potential zitha kuwoneka mu Chithunzi 4a. Pa nthawi yoyika 6, mphamvu yayikulu ya nanocomposite imafika -550 mV poyerekeza ndi saturated calomel electrode, ndipo mphamvu ya nanocomposite yomwe imayikidwa ndi factor ya 6 ndi yotsika kwambiri kuposa ya nanocomposite pansi pa mikhalidwe ina. Chifukwa chake, ma nanocomposites a NiS/TiO2 omwe adapezeka pambuyo pa ma 6 deposition cycles adapereka chitetezo chabwino kwambiri cha cathodic cha 304 stainless steel.
Kusintha kwa OCP kwa ma electrode 304 osapanga dzimbiri okhala ndi ma nanocomposites a NiS/TiO2 (a) ndi ma nanocomposites a Ag/NiS/TiO2 (b) okhala ndi komanso opanda kuwala (λ > 400 nm).
Monga momwe zasonyezedwera pa chithunzi 4b, mphamvu ya open circuit ya 304 stainless steel ndi Ag/NiS/TiO2 nanocomposites inachepa kwambiri pamene inayikidwa pa kuwala. Pambuyo poika pamwamba pa nanoparticles zasiliva, mphamvu ya open circuit inachepa kwambiri poyerekeza ndi nanowires za TiO2 zoyera. Mphamvu ya nanocomposite ya NiS/TiO2 ndi yoipa kwambiri, zomwe zikusonyeza kuti mphamvu yoteteza ya cathodic ya TiO2 imakula bwino kwambiri pambuyo poti nanoparticles za Ag zaikidwa. Mphamvu ya open circuit inakula mofulumira kumapeto kwa kuonekera, ndipo poyerekeza ndi saturated calomel electrode, mphamvu ya open circuit inatha kufika -580 mV, yomwe inali yotsika kuposa ya 304 stainless steel (-180 mV). Zotsatirazi zikusonyeza kuti nanocomposite ili ndi mphamvu yosungira mphamvu zodabwitsa pambuyo poti tinthu ta siliva taikidwa pamwamba pake. Pa chithunzi 4b ikuwonetsanso momwe kuchuluka kwa siliva nitrate kumakhudzira mphamvu ya open circuit. Pa kuchuluka kwa siliva nitrate ya 0.1 M, mphamvu yoletsa poyerekeza ndi saturated calomel electrode imafika -925 mV. Pambuyo pa nthawi zinayi zogwiritsidwa ntchito, mphamvuyo inakhalabe pamlingo pambuyo pa nthawi yoyamba yogwiritsidwa ntchito, zomwe zikusonyeza kukhazikika kwabwino kwa nanocomposite. Chifukwa chake, pa kuchuluka kwa nitrate yasiliva ya 0.1 M, nanocomposite ya Ag/NiS/TiO2 yomwe yapezeka imakhala ndi chitetezo chabwino kwambiri cha cathodic pa chitsulo chosapanga dzimbiri cha 304.
Kuyika kwa NiS pamwamba pa ma nanowaya a TiO2 kumawonjezeka pang'onopang'ono ndi nthawi yowonjezera ya NiS. Kuwala kooneka kukafika pamwamba pa nanowaya, malo ambiri ogwira ntchito a nickel sulfide amasangalala kupanga ma elekitironi, ndipo kuthekera kwa photoionization kumachepa kwambiri. Komabe, pamene nickel sulfide nanoparticles ikayikidwa kwambiri pamwamba, nickel sulfide yolimbikitsidwa imachepa m'malo mwake, zomwe sizimathandizira kuyamwa kwa kuwala. Tinthu ta siliva titayikidwa pamwamba, chifukwa cha plasmon resonance effect ya tinthu ta siliva pamwamba, ma elekitironi opangidwa amasamutsidwa mwachangu pamwamba pa 304 stainless steel, zomwe zimapangitsa kuti chitetezo cha cathodic chikhale chabwino kwambiri. Tinthu ta siliva tikakhala tambirimbiri pamwamba, tinthu ta siliva timakhala malo obwerezabwereza a ma photoelectron ndi mabowo, zomwe sizimathandizira kupanga ma photoelectron. Pomaliza, ma nanocomposites a Ag/NiS/TiO2 angapereke chitetezo chabwino kwambiri cha cathodic cha 304 stainless steel pambuyo pa 6-fold nickel sulfide deposition pansi pa 0.1 M silver nitrate.
Kuchuluka kwa mphamvu ya photocurrent kumayimira mphamvu yolekanitsa ma elekitironi ndi mabowo opangidwa ndi photo, ndipo kuchuluka kwa mphamvu ya photocurrent, mphamvu yolekanitsa ma elekitironi ndi mabowo opangidwa ndi photo imakulanso. Pali maphunziro ambiri omwe akusonyeza kuti NiS imagwiritsidwa ntchito kwambiri popanga zinthu zopanga photocatalytic kuti ikonze mphamvu ya photoelectric ya zinthuzo komanso kulekanitsa mabowo15,16,17,18,19,20. Chen et al. adaphunzira za graphene yopanda zitsulo ndi g-C3N4 composites zomwe zidasinthidwa ndi NiS15. Mphamvu yayikulu ya photocurrent ya g-C3N4/0.25%RGO/3%NiS yosinthidwa ndi 0.018 μA/cm2. Chen et al. adaphunzira za CdSe-NiS yokhala ndi mphamvu ya photocurrent ya pafupifupi 10 µA/cm2.16. Liu et al. adapanga CdS@NiS composite yokhala ndi mphamvu ya photocurrent ya 15 µA/cm218. Komabe, kugwiritsa ntchito NiS poteteza photocathode sikunanenedwebe. Mu kafukufuku wathu, kuchuluka kwa mphamvu ya TiO2 pa photocurrent kunawonjezeka kwambiri chifukwa cha kusintha kwa NiS. Pa chithunzi 5 chikuwonetsa kusintha kwa kuchuluka kwa mphamvu ya photocurrent ya 304 stainless steel ndi nanocomposites pansi pa kuwala kowoneka komanso popanda kuunikira. Monga momwe zasonyezedwera pa chithunzi 5a, kuchuluka kwa mphamvu ya NiS/TiO2 nanocomposite kumawonjezeka mofulumira panthawi yomwe kuwala kumayatsidwa, ndipo kuchuluka kwa mphamvu ya photocurrent ndi kwabwino, zomwe zikusonyeza kuyenda kwa ma elekitironi kuchokera ku nanocomposite kupita pamwamba kudzera mu electrochemical workstation. 304 stainless steel. Pambuyo pokonza ma nickel sulfide composites, kuchuluka kwa mphamvu ya photocurrent kumakhala kwakukulu kuposa kwa ma nanowires a TiO2 oyera. Kuchuluka kwa mphamvu ya photocurrent ya NiS kumafika pa 220 μA/cm2, komwe ndi kokwera nthawi 6.8 kuposa kwa ma nanowires a TiO2 (32 μA/cm2), pamene NiS imamizidwa ndikuyikidwa nthawi 6. Monga momwe zasonyezedwera pa chithunzi. 5b, kuchuluka kwa kuwala kwa dzuwa pakati pa nanocomposite ya Ag/NiS/TiO2 ndi chitsulo chosapanga dzimbiri cha 304 kunali kwakukulu kwambiri kuposa pakati pa TiO2 yoyera ndi nanocomposite ya NiS/TiO2 ikayatsidwa pansi pa nyali ya xenon. Pa chithunzi 5b, chikuwonetsanso momwe kuchuluka kwa AgNO kumakhudzira kuchuluka kwa kuwala kwa dzuwa panthawi yochepetsa kuwala. Pa kuchuluka kwa nitrate yasiliva ya 0.1 M, kuchuluka kwake kwa kuwala kwa dzuwa kumafika 410 μA/cm2, komwe ndi kokwera nthawi 12.8 kuposa kwa ma nanowire a TiO2 (32 μA/cm2) ndi kokwera nthawi 1.8 kuposa kwa ma nanocomposites a NiS/TiO2. Munda wamagetsi wa heterojunction umapangidwa pa mawonekedwe a nanocomposite a Ag/NiS/TiO2, omwe amathandizira kulekanitsa ma elekitironi opangidwa ndi kuwala kuchokera ku mabowo.
Kusintha kwa kuchuluka kwa kuwala kwa electrode ya chitsulo chosapanga dzimbiri ya 304 yokhala ndi (a) NiS/TiO2 nanocomposite ndi (b) Ag/NiS/TiO2 nanocomposite yokhala ndi kuwala kopanda (λ > 400 nm).
Motero, pambuyo pa kumiza kwa nickel sulfide kwa ma cycle 6 mu 0.1 M siliva nitrate wokhazikika, kuchuluka kwa photocurrent pakati pa Ag/NiS/TiO2 nanocomposites ndi 304 stainless steel kumafika pa 410 μA/cm2, komwe ndi kwakukulu kuposa kwa saturated calomel. ma electrodes amafika pa -925 mV. Pansi pa izi, 304 stainless steel kuphatikiza ndi Ag/NiS/TiO2 kungapereke chitetezo chabwino kwambiri cha cathodic.
Pa chithunzi 6 chikuwonetsa zithunzi za maikulosikopu ya ma electron pamwamba pa ma nanowaya oyera a titanium dioxide, ma nanoparticles a nickel sulfide, ndi ma nanoparticles asiliva pansi pa mikhalidwe yabwino. Pa chithunzi 6a, d chikuwonetsa ma nanowaya oyera a TiO2 omwe amapezeka ndi anodization ya gawo limodzi. Kufalikira kwa pamwamba pa ma nanowaya a titanium dioxide ndi kofanana, kapangidwe ka ma nanowaya ali pafupi wina ndi mnzake, ndipo kufalikira kwa kukula kwa pore ndi kofanana. Zithunzi 6b ndi e ndi ma micrographs a ma electron a titanium dioxide pambuyo pa kulowetsedwa kasanu ndi kamodzi ndi kuikidwa kwa ma nickel sulfide composites. Kuchokera pachithunzi cha maikulosikopu cha ma electron chomwe chakulitsidwa nthawi 200,000 mu Chithunzi 6e, zitha kuwoneka kuti ma nanoparticles a nickel sulfide composite ndi ofanana ndipo ali ndi tinthu tating'onoting'ono tating'ono tomwe tili pafupifupi 100–120 nm m'mimba mwake. Ma nanoparticles ena amatha kuwoneka pamalo a nanowaya, ndipo ma nanowaya a titanium dioxide amawonekera bwino. Pa chithunzi 6b ndi e ndi ma micrographs a ma electron a titanium dioxide atayikidwa kasanu ndi kamodzi ndi kuikidwa kwa ma composites a nickel sulfide. Kuchokera pachithunzi cha maikulosikopu cha ma electron microscopic chomwe chakulitsidwa nthawi 200,000 mu Chithunzi 6e, zitha kuwoneka kuti ma nanoparticles a nickel sulfide composite ndi ofanana ndipo ali ndi tinthu tating'onoting'ono tating'ono tomwe tili pafupifupi 100–120 nm m'mimba mwake. Ma nanoparticles ena amatha kuwoneka pamalo a nanowaya, ndipo ma nanowaya a titanium dioxide amawonekera bwino. Pa chithunzi 6b ndi e ndi ma micrographs a ma electron a titanium dioxide atayikidwa kasanu ndi kamodzi ndi kuyikidwa kwa ma composites a nickel sulfide. Kuchokera pachithunzi cha maikulosikopu cha ma electron microscopic chomwe chakulitsidwa nthawi 200,000 mu Chithunzi 6e, zitha kuwoneka kuti ma nanoparticles a nickel sulfide composite ndi ofanana ndipo ali ndi tinthu tating'onoting'ono tating'onoting'ono tating'onoting'ono tating'onoting'ono tating'onoting'ono tating'onoting'ono tating'onoting' 6c,f ikuwonetsa zithunzi za ma electron microscopic a NiS/TiO2 nanocomposites pamlingo wa AgNO wa 0.1 M. Poyerekeza ndi Zithunzi 6b ndi Chithunzi 6e, Chithunzi 6c ndi Chithunzi 6f zikuwonetsa kuti ma nanoparticles a Ag amaikidwa pamwamba pa zinthu zophatikizika, ndi ma nanoparticles a Ag omwe amagawidwa mofanana ndi mainchesi pafupifupi 10 nm. Pa chithunzi 7 ikuwonetsa gawo lozungulira la ma nanofilms a Ag/NiS/TiO2 omwe adayikidwa mu ma cycle 6 a NiS dip deposition pamlingo wa AgNO3 wa 0.1 M. Kuchokera pazithunzi zokulitsa kwambiri, makulidwe a filimu yoyesedwa anali 240-270 nm. Chifukwa chake, ma nanoparticles a nickel ndi siliva sulfide amasonkhanitsidwa pamwamba pa ma nanowaya a TiO2.
TiO2 yoyera (a, d), NiS/TiO2 nanocomposites yokhala ndi ma cycle 6 a NiS dip deposition (b, e) ndi Ag/NiS/NiS yokhala ndi ma cycle 6 a NiS dip deposition pa 0.1 M AgNO3 SEM zithunzi za TiO2 nanocomposites (c, e).
Gawo lopingasa la ma nanofilms a Ag/NiS/TiO2 linayikidwa mu ma cycle 6 a NiS dip deposition pa AgNO3 concentration ya 0.1 M.
Pa chithunzi 8 chikuwonetsa kufalikira kwa zinthu pamwamba pa pamwamba pa nanocomposites za Ag/NiS/TiO2 zomwe zapezeka kuchokera ku ma cycle 6 a nickel sulfide dip deposition pa silver nitrate concentration ya 0.1 M. Kufalikira kwa zinthu pamwamba pa kusonyeza kuti Ti, O, Ni, S ndi Ag zinapezeka pogwiritsa ntchito energy spectroscopy. Ponena za kuchuluka kwa zinthu, Ti ndi O ndi zinthu zomwe zimapezeka kwambiri pakugawidwa, pomwe Ni ndi S zili pafupifupi zofanana, koma kuchuluka kwawo ndi kochepa kwambiri kuposa Ag. Zingatsimikizidwenso kuti kuchuluka kwa nanoparticles zasiliva zomwe zili pamwamba ndi kwakukulu kuposa kwa nickel sulfide. Kufalikira kofanana kwa zinthu pamwamba kumasonyeza kuti nickel ndi sulfide zasiliva zimagwirizanitsidwa mofanana pamwamba pa nanowaya za TiO2. Kusanthula kwa X-ray photoelectron spectroscopic kunachitikanso kuti kufufuze kapangidwe kake ndi momwe zinthu zimamangidwira.
Kugawa kwa zinthu (Ti, O, Ni, S, ndi Ag) za Ag/NiS/TiO2 nanocomposites pa AgNO3 concentration ya 0.1 M kwa ma cycle 6 a NiS dip deposition.
Pa chithunzi 9 chikuwonetsa ma XPS spectra a Ag/NiS/TiO2 nanocomposites omwe amapezeka pogwiritsa ntchito ma cycle 6 a nickel sulfide deposition powamiza mu 0.1 M AgNO3, pomwe chithunzi 9a ndiye full spectrum, ndipo ma spectra ena onse ndi high-resolution spectra ya zinthuzo. Monga momwe tikuonera kuchokera ku full spectrum mu Chithunzi 9a, ma absorption peaks a Ti, O, Ni, S, ndi Ag adapezeka mu nanocomposite, zomwe zimatsimikizira kukhalapo kwa zinthu zisanuzi. Zotsatira za mayeso zinali zogwirizana ndi EDS. Nsonga yochulukirapo mu Chithunzi 9a ndi carbon peak yomwe imagwiritsidwa ntchito kukonza mphamvu yomangirira ya chitsanzocho. Pa chithunzi 9b chikuwonetsa high resolution energy spectrum ya Ti. Ma absorption peaks a 2p orbitals ali pa 459.32 ndi 465 eV, omwe amagwirizana ndi absorption ya Ti 2p3/2 ndi Ti 2p1/2 orbitals. Ma peak awiri oyamwa amatsimikizira kuti titaniyamu ili ndi Ti4+ valence, yomwe ikugwirizana ndi Ti mu TiO2.
Ma spectra a XPS a muyeso wa Ag/NiS/TiO2 (a) ndi ma spectra a XPS okhala ndi resolution yapamwamba a Ti2p(b), O1s(c), Ni2p(d), S2p(e), ndi Ag 3d(f).
Pa chithunzi 9d chikuwonetsa mphamvu ya Ni yapamwamba kwambiri yokhala ndi nsonga zinayi zoyamwitsa za Ni 2p orbital. Nsonga zoyamwitsa pa 856 ndi 873.5 eV zikugwirizana ndi Ni 2p3/2 ndi Ni 2p1/2 8.10 orbitals, komwe nsonga zoyamwitsa zili za NiS. Nsonga zoyamwitsa pa 881 ndi 863 eV ndi za nickel nitrate ndipo zimayambitsidwa ndi nickel nitrate reagent panthawi yokonzekera chitsanzo. Pa chithunzi 9e chikuwonetsa S-spectrum yapamwamba kwambiri. Nsonga zoyamwitsa za S 2p orbitals zili pa 161.5 ndi 168.1 eV, zomwe zikugwirizana ndi S 2p3/2 ndi S 2p1/2 orbitals 21, 22, 23, 24. Nsonga ziwirizi ndi za nickel sulfide compounds. Nsonga zoyamwitsa pa 169.2 ndi 163.4 eV ndi za sodium sulfide reagent. Pa chithunzi 9e chikuwonetsa S-spectrum yapamwamba kwambiri. Nsonga zoyamwitsa za S 2p orbitals zili pa 161.5 ndi 168.1 eV, zomwe zikugwirizana ndi S 2p3/2 ndi S 2p1/2 orbitals 21, 22, 23, 24. Nsonga ziwirizi ndi za nickel sulfide compounds. Nsonga zoyamwitsa pa 169.2 ndi 163.4 eV ndi za sodium sulfide reagent. Pa chithunzi 9e 9f ikuwonetsa mtundu wa Ag spectrum wapamwamba kwambiri momwe nsonga za siliva zoyamwa za orbital 3d zili pa 368.2 ndi 374.5 eV, motsatana, ndipo nsonga ziwiri zoyamwa zimagwirizana ndi njira zoyamwa za Ag 3d5/2 ndi Ag 3d3/212, 13. Nsonga m'malo awiriwa zimatsimikizira kuti tinthu tating'onoting'ono ta siliva tilipo mu mkhalidwe wa siliva wa elemental. Chifukwa chake, tinthu tating'onoting'ono ta nanocomposites timapangidwa makamaka ndi Ag, NiS ndi TiO2, zomwe zidatsimikiziridwa ndi X-ray photoelectron spectroscopy, zomwe zidatsimikizira kuti tinthu tating'onoting'ono ta nickel ndi siliva sulfide zidaphatikizidwa bwino pamwamba pa tinthu ta TiO2 nanowires.
Pa chithunzi 10 chikuwonetsa ma spectra owunikira a UV-VIS a ma nanowaya a TiO2 okonzedwa kumene, ma nanocomposites a NiS/TiO2, ndi ma nanocomposites a Ag/NiS/TiO2. Zitha kuwoneka kuchokera pachithunzichi kuti malire oyamwa a ma nanowaya a TiO2 ndi pafupifupi 390 nm, ndipo kuwala komwe kumayamwa kumakhala kwakukulu m'dera la ultraviolet. Zitha kuwoneka kuchokera pachithunzichi kuti pambuyo pa kuphatikiza ma nanowaya a nickel ndi siliva sulfide pamwamba pa ma nanowaya a titanium dioxide 21, 22, kuwala komwe kumayamwa kumafalikira m'dera lowala looneka. Nthawi yomweyo, nanocomposite imawonjezera kuyamwa kwa UV, komwe kumalumikizidwa ndi kusiyana kochepa kwa nickel sulfide. Kusiyana kwa band kumachepa, chotchinga champhamvu cha kusintha kwamagetsi chimachepa ndipo kuchuluka kwa kugwiritsa ntchito kuwala kumakwera. Pambuyo pophatikiza pamwamba pa NiS/TiO2 ndi ma nanowaya asiliva, mphamvu ya kuyamwa ndi kutalika kwa kuwala sikunakwere kwambiri, makamaka chifukwa cha zotsatira za plasmon resonance pamwamba pa ma nanowaya asiliva. Kutalika kwa mayamwidwe a ma nanowaya a TiO2 sikukwera kwambiri poyerekeza ndi kusiyana kwa gulu laling'ono la ma nanowaya a composite NiS. Mwachidule, pambuyo pa ma nanowaya a nickel sulfide ndi siliva pamwamba pa ma nanowaya a titanium dioxide, mawonekedwe ake oyamwitsa kuwala amakula kwambiri, ndipo kuchuluka kwa kuyamwa kwa kuwala kumawonjezeka kuchokera ku ultraviolet kupita ku kuwala kowoneka, zomwe zimapangitsa kuti ma nanowaya a titanium dioxide agwiritsidwe ntchito bwino, zomwe zimapangitsa kuti zinthuzo zizitha kupanga ma photoelectron.
Ma spectra owunikira a UV/Vis a ma nanowaya atsopano a TiO2, ma nanocomposites a NiS/TiO2, ndi ma nanocomposites a Ag/NiS/TiO2.
Pa chithunzi 11 chikuwonetsa momwe kuwala kwa Ag/NiS/TiO2 nanocomposites kumagwirira ntchito pogwiritsa ntchito kuwala kowala. Kutengera momwe ma nanoparticles asiliva, nickel sulfide, ndi gulu loyendetsa la titanium dioxide zimagawidwira, mapu otheka a momwe kuwala kumagwirira ntchito akusonyezedwera. Chifukwa mphamvu ya gulu loyendetsa la nanosilver ndi yoyipa poyerekeza ndi nickel sulfide, ndipo mphamvu ya gulu loyendetsa la nickel sulfide ndi yoyipa poyerekeza ndi titanium dioxide, njira yoyendera ma elekitironi ndi pafupifupi Ag→NiS→TiO2→304 chitsulo chosapanga dzimbiri. Kuwala kukayatsidwa pamwamba pa nanocomposite, chifukwa cha mphamvu ya plasmon resonance ya nanosilver, nanosilver imatha kupanga mabowo ndi ma elekitironi opangidwa ndi photochemical mwachangu, ndipo ma elekitironi opangidwa ndi photochemical amasuntha mwachangu kuchokera pamalo a valence band kupita pamalo a gulu loyendetsa chifukwa cha kukwiya. Titanium dioxide ndi nickel sulfide. Popeza mphamvu ya ma nanoparticles asiliva ndi yoipa kwambiri kuposa ya nickel sulfide, ma elekitironi mu TS ya ma nanoparticles asiliva amasinthidwa mwachangu kukhala TS ya nickel sulfide. Mphamvu ya nickel sulfide yoyendetsa ndi yoipa kwambiri kuposa ya titanium dioxide, kotero ma elekitironi a nickel sulfide ndi mphamvu ya siliva zimasonkhana mwachangu mu CB ya titanium dioxide. Ma elekitironi opangidwa ndi photogenerated amafika pamwamba pa 304 stainless steel kudzera mu titanium matrix, ndipo ma elekitironi olemerawo amagwira nawo ntchito yochepetsa mpweya wa cathodic wa 304 stainless steel. Njirayi imachepetsa cathodic reaction ndipo nthawi yomweyo imaletsa anodic dissolving reaction ya 304 stainless steel, motero imazindikira cathodic protection ya 304 stainless steel. Chifukwa cha kupangika kwa magetsi a heterojunction mu Ag/NiS/TiO2 nanocomposite, mphamvu ya conductive ya nanocomposite imasunthidwa kukhala malo oipa kwambiri, zomwe zimapangitsa bwino kwambiri chitetezo cha cathodic cha 304 stainless steel.
Chithunzi chojambula cha njira yotsutsana ndi dzimbiri ya Ag/NiS/TiO2 nanocomposites mu kuwala kooneka.
Mu ntchito iyi, tinthu tating'onoting'ono ta nickel ndi siliva sulfide tinapangidwa pamwamba pa ma nanowaya a TiO2 pogwiritsa ntchito njira yosavuta yoyeretsera ndi yochepetsera kuwala. Kafukufuku wotsatira wokhudza chitetezo cha cathodic cha ma nanocomposites a Ag/NiS/TiO2 pa chitsulo chosapanga dzimbiri cha 304 unachitika. Kutengera ndi mawonekedwe a mawonekedwe, kusanthula kapangidwe kake ndi kusanthula kwa mawonekedwe a kuyamwa kwa kuwala, mfundo zazikulu izi zidapangidwa:
Ndi ma impregnation-deposition cycles angapo a nickel sulfide a 6 ndi kuchuluka kwa siliva nitrate kuti ichepetse 0.1 mol/l, ma nanocomposites a Ag/NiS/TiO2 omwe adapezeka anali ndi mphamvu yabwino yoteteza cathodic pa chitsulo chosapanga dzimbiri cha 304. Poyerekeza ndi saturated calomel electrode, chitetezo chimafika -925 mV, ndipo chitetezo chimafika 410 μA/cm2.
Munda wamagetsi wa heterojunction umapangidwa pa Ag/NiS/TiO2 nanocomposite interface, zomwe zimapangitsa kuti mphamvu yolekanitsa ma elekitironi ndi mabowo opangidwa ndi photogenerated ikhale yowonjezereka. Nthawi yomweyo, kugwiritsa ntchito bwino kuwala kumawonjezeka ndipo kuchuluka kwa kuwala kumawonjezeka kuchokera kudera la ultraviolet kupita kudera looneka. Nanocomposite idzakhalabe ndi mawonekedwe ake oyambirira ndi kukhazikika bwino pambuyo pa ma cycle anayi.
Ma nanocomposites a Ag/NiS/TiO2 okonzedwa mwachiyembekezo ali ndi malo ofanana komanso okhuthala. Nickel sulfide ndi siliva nanoparticles zimagwirizanitsidwa mofanana pamwamba pa ma nanowaya a TiO2. Ma nanoparticles a cobalt ferrite ndi siliva ndi oyera kwambiri.
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