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Elektrohemijsko taloženje niobijuma iz fluoridnih rastvora i hloroaluminatnih rastopa na staklastom ugljeniku, platini i zlatu / Electrochemical deposition of niobium from fluoride solution and chloroaluminate melts on glassy carbon, platinum and gold

<p>Cilj ovog rada bio je da se ustanovi da li dolazi do elektrohemijskog taloženja&nbsp; niobijuma i aluminijuma iz hloroaluminatnih rastopa obogaćenih niobijumom na podlogama od staklastog&nbsp; ugljenika, platine i zlata. Nadalje, ako dolazi do rečenog&nbsp; taloženja, da li pri tome dolazi i do formiranja legura niobijuma sa izabranim podlogama kao i da li dolazi do formiranja legura niobijuma sa zajednički taloženim aluminijumom. I na kraju,&nbsp; cilj je&nbsp; bio da se navedeni fenomeni ostvare na &scaron;to nižim temperaturama.</p><p>Nb&nbsp; i&nbsp; Al&nbsp; su elektrohemijski taloženi na staklastom ugljeniku, platini i zlatu pri 200&nbsp; &deg;C, pod atmosferom argona, iz rastopa napravljenog od ekvimolarne sme&scaron;e AlCl<sub>3</sub> + NaCl kome&nbsp; je dodat niobijum.</p><p>U istraživanjima su kori&scaron;ćene: linearna&nbsp; i&nbsp; ciklička voltametrija, metoda potenciodinamičke polarizacione krive, metoda &bdquo;otvorenog kola&ldquo;,&nbsp; hronoamperometrija,&nbsp; SEM,&nbsp; EDS, AFM&nbsp; i XRD analiza.</p><p>Elektrohemijsko taloženje Nb i Al iz primenjenih rastopa pri potpotencijalima uočeno je na podlozi od zlata. Taloženje niobijuma pri potpotencijalima na zlatu je novost, a taloženje Al na zlatu pri&nbsp; potpotencijalima poznato je od ranije. Elektrotaloženje&nbsp; Al&nbsp; i&nbsp; Nb&nbsp; iz primenjenih rastopa pri potpotencijalu na zlatu prethodi procesima elektrotaloženja niobijuma i aluminijuma pri natpotencijalima.&nbsp; Rezultat ovih procesa su Nb/Au i Al/Au legure nastale zajedničkim taloženjem i interdifuzijom istaloženog Nb, odnosno&nbsp; Al i podloge&nbsp; -&nbsp; zlata (AlAu,&nbsp; AlAu<sub>2</sub> , AlAu<sub>4</sub>, AlNb<sub>2</sub> , AlNb<sub>3</sub> , Au<sub>2</sub>Nb, Au<sub>2</sub>Nb<sub>3</sub> , AuNb<sub>3</sub> , AlNb<sub>3</sub>).</p><p>Elektrohemijsko taloženje Nb iz primenjenih rastopa pri potpotencijalima uočeno je na platini i prethodi procesima elektrotaloženja&nbsp; Nb&nbsp; i&nbsp; Al. Rezultat su formirane Nb/Pt legure nastale interdifuzijom&nbsp; istaloženog Nb i podloge&nbsp; -&nbsp; platine (Nb<sub>3</sub>Pt). Pri natpotencijalima aluminijuma na&nbsp; platini dolazi do taloženja metalnog niobijuma, metalnog aluminijuma i zajedničkog taloženja Nb i Al. Kao posledica&nbsp; ovih procesa dolazi i do formiranja legura (AlNb<sub>3</sub>, Al<sub>3</sub>Pt<sub>5</sub> ,&nbsp; Nb<sub>3</sub>Pt).</p><p>Elektrohemijsko taloženje niobijuma iz primenjenih rastopa na izabranim podlogama odigrava se na potencijalima koji su pozitivniji od potencijala&nbsp; elektrotaloženja aluminijuma.</p><p>Sve dobijene legure formirane su pri temperaturi od 200 &deg;C &scaron;to je nekoliko stotina stepeni niže od odgovarajućih temperatura potrebnih da se formiraju termičkim putem.&nbsp;</p> / <p>The aim of this study was to establish electrodeposition of niobium and aluminium from chloroaluminate melt (AlCl<sub>3</sub> + NaCl) enriched with niobium onto gold, platinum and glassy carbon substrates. Furthermore, if such deposition is shown to occur,&nbsp; to&nbsp; assess if it can lead to formation ofniobium alloys with chosen substrates or&nbsp; formation of Nb/Al alloys as a result of codeposition. And finally, if the deposition is indeed confirmed,&nbsp; to&nbsp; establish the lowest operational temperature at which it is possible.</p><p>Niobium and aluminium were electrodeposited onto glassy carbon, gold and platinum at&nbsp; 200 &deg;C, under an argon atmophere&nbsp; from the melt made of&nbsp; equimolar mixture AlCl<sub>3</sub> + NaCl with niobium being added.</p><p>Research methods used were:&nbsp; cyclic voltammetry, potentiodynamic polarization curves, &quot;open circuit&rdquo;, chronoamperometry,&nbsp; SEM,&nbsp; EDS, AFM and&nbsp; XRD&nbsp; analysis. Underpotential deposition of&nbsp; Nb&nbsp; and Al&nbsp; from the melt onto gold substrate was observed. Of the two, niobium deposition is a novelty, while alumininum deposition has been previously studied.&nbsp; Underpotential deposition of&nbsp; NB and Al onto gold from given melt precedes the overpotential deposition of aluminium and niobium onto gold. The result of these processes are Nb/Au and Al/Au alloys formed by codeposition of the two metals&nbsp; and&nbsp; interdiffusion between the Nb and Al deposits and the substrate -gold (AlAu, AlAu<sub>2</sub>, AlAu<sub>4</sub>, AlNb<sub>2</sub>, AlNb<sub>3</sub>,&nbsp; Au<sub>2</sub>Nb, Au<sub>2</sub>Nb<sub>3</sub>, AuNb<sub>3</sub>, AlNb<sub>3</sub>). Underpotential deposition of niobium onto platinum from used melts was recorded and it precedes the&nbsp; processes of overpotential deposition of niobium and aluminium. The result is formation of Nb/Pt alloys as a consequence of&nbsp; interdiffusion between the substrate and the deposited Nb (Nb<sub>3</sub>Pt). The potentials more negative than the aluminium deposition potential in the used system lead to deposition of niobium and aluminium&nbsp; individually and jointly. Thus, a number of alloys are formed (AlNb<sub>3</sub>, Al<sub>3</sub>Pt<sub>5</sub>, Nb<sub>3</sub>Pt).&nbsp; Niobium electrodeposition onto chosen substrates from the melt applied takes place at potentials which are more positive than the potential of electrodeposition of aluminium. Formation of&nbsp; the&nbsp; obtained alloys occurred at a temperature of 200 &deg;C which is several hundred degrees lower than the temperatures needed for their formation by thermal methods.</p>

Identiferoai:union.ndltd.org:uns.ac.rs/oai:CRISUNS:(BISIS)104330
Date18 May 2017
CreatorsVukićević Nataša
ContributorsJovanović Ljiljana, Cvetković Vesna, Vaštag Đenđi, Stevanović Jasmina
PublisherUniverzitet u Novom Sadu, Prirodno-matematički fakultet u Novom Sadu, University of Novi Sad, Faculty of Sciences at Novi Sad
Source SetsUniversity of Novi Sad
LanguageSerbian
Detected LanguageEnglish
TypePhD thesis

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