Elecrochemical Behaviour of Zinc on Copper and on Vitreous. Carbon Electrodes. The Influence of Gluconate

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1 Portuglie Eletrohimi At 21 (2003) PORTUGALIAE ELECTROCHIMICA ACTA Elerohemil Behviour of Zin on Copper nd on Vitreous Cron Eletrodes. The Influene of Gluonte J. Torrent-Burgués *, E. Guus Group of Eletrohemistry of Mterils, Deprtment of Chemil Engineering, Universitt Politèni de Ctluny, C/ Colom 1, 08222, Terrss, Spin Reeived 7 Jnury 2003; epted in revised form 9 My 2003 Astrt The zin eletrohemil ehviour from sulphte nd sulphte-gluonte ths ws studied oth on vitreous ron nd opper eletrode. The voltmmetri response depends on the omplexing gent onentrtion, the eletrode mteril, the ph nd the thodi potentil limit. The redution of zin ions proeeds with hydrogen evolution, nd t less negtive potentils on the opper eletrode thn on the vitreous ron eletrode, speilly in sene of gluonte. Gluonte dereses the effiieny of the proess. On the other hnd, gluonte fvours zin eletrodeposition on vitreous ron ut retrds it on opper. Keywords: zin, vitreous ron, opper eletrode, gluonte, sulphte ths. Introdution Zin is widely used in eletrometllurgy. Zin eletrodeposition hs usully een studied using vitreous ron eletrode in highly idi ths of oth hloride nd sulphte. Other eletrodes s zin or pltinum hve lso een used. Few studies hve reported the influene of omplexing gents nd of slightly idi ph on the eletrodeposition proess of zin. The eletrodeposition of zin from sulphte ths ws studied y Lmping nd Keefe [1], nd y Despi nd Pvlovi [2] on pltinum, gold nd grphite * Corresponding uthor. E-mil ddress: jtorrent@eq.up.es.

2 eletrodes from uffered solutions t ph = 3.55, nd y Beshore et l. [3] on vitreous ron eletrode in high idi th. Chet nd Wirt [4] studied zin eletrodeposition on zin eletrode from highly idi sulphte eletrolytes, Muñoz et l. [5] studied zin eletrodeposition on vitreous ron eletrode from hloride or sulphte ths t ph lose to 3, nd Teixeir et l. [6] on pltinum. Other reported medi for zin eletrodeposition re solutions of hloride [7, 8], zinte [9], n orgni th [10], or ommeril umultor solutions [11]. Underpotentil deposition of zin on Pt(111) in lkline solution ws studied y Igrshi et l. [12]. Formtion of zin films using eletro-plting versus eletroless-plting ws desried y Med nd Nishio [13]. Gluonte is omplexing gent tht hs een used in eletrodeposition studies of other metls suh s Sn [14]. Zin ions re lso omplexed y gluonte nd this omplexing tion n influene the zin eletrodeposition. The gluonte ions ompete with the sulphte ions for omplexing the zin ions. In this study the eletrohemil ehviour of zin in the presene of gluonte from severl slightly idi sulphte ths is presented, in order to determine the influene of this omplexing gent on the eletrohemil ehviour of zin. The influene of the sustrte is tested using vitreous ron nd opper eletrode, nd no referenes hve een found in the literture out the use of opper eletrode. The zin eletrohemil ehviour is lso ompred with tht of zin from other ths, s well s with tht of other metls from sulphte/gluonte ths. Experimentl The eletrohemil mesurements were performed in three-eletrode ell using rod of vitreous ron or opper s the working eletrode (re = m 2 ), pltinum wire s the ounter eletrode nd Ag/AgCl/NCl (1 M) s the referene eletrode, inserted in Luggin pillry. All potentils reported in the text re referred to this eletrode. A miroomputer-ontrolled AUTOLAB PSTAT20 ws used s potentiostt. Different sets of yli voltmmetri 180

3 experiments were performed running only one yle in eh experiment nd snning t first towrds negtive potentils, until thodi limit potentil E l. Anodi stripping voltmmetri experiments were performed immeditely fter potentiostti deposition without removing the eletrode from the ell. The nodi stripping voltmmetry ws lwys rried out strting t n initil potentil t whih deposition did not our nd snning to n nodi potentil limit where the zin is totlly dissolved. The working temperture ws of 25 ºC. The hemils used were ZnSO 4 7H 2 O, sodium gluonte (NC 6 H 11 O 7 ) nd N 2 SO 4 (nlytil grde). All solutions were freshly prepred with wter, first distilled nd then treted with Millipore Milli Q system. The sulphte th ontined 0.01 M ZnSO 4 nd 1 M N 2 SO 4 s supporting eletrolyte (ph of the th 5.1). The gluonte/sulphte th ontined 0.01 M ZnSO 4, 1 M N 2 SO 4 s supporting eletrolyte nd 0.2 M sodium gluonte s the omplexing gent (ph of the th 5.7). The working ph in the experiments ws tht of the th or ws djusted to 4 using 1 M H 2 SO 4. Before nd during eh experiment the solution ws deerted with rgon. The working eletrode ws polished mehnilly efore eh run with 3.75 nd 1.87 µm lumin powder, lened ultrsonilly nd followed y short eletrohemil onditioning pplying potentil of -200 mv during 20 s. Results nd Disussion The voltmmetri response depends on the presene or not of the omplexing gent, on the eletrode mteril nd on the ph. The nodi sn lso depends on the thodi potentil limit. Blnk solutions Previously to the zin studies, voltmmetri experiments were done in lnk solutions of sulphte, either in the sene or in the presene of gluonte. Fig. 1 shows the results of these experiments on the opper eletrode. It is seen tht hydrogen evolution is fvoured t lower ph, s is usul, nd in the presene of 181

4 gluonte. The hydrogen formtion is lso more fvoured on the opper thn on the vitreous ron eletrode. Asene of gluonte Fig. 2 shows the voltmmetri responses, t sn rte of 50 mv s -1, of sulphte th ontining zin ions t ph 4, using oth opper or vitreous ron eletrode. It is seen tht zin deposition shifts to more positive potentils for the opper eletrode, s well s hydrogen formtion. Then, while the eletrodeposition proess ours with signifint overpotentil on the vitreous ron eletrode, it ours with no or smll overpotentil on opper. The thodi sn lso shows, for the opper eletrode, signifint pitive urrent t potentils where, neither deposition nor hydrogen formtion, ours (see Figs. 1 nd 2). 0-0,05 i / ma -0,1-0,15-1,6-1,4-1,2-1 -0,8-0,6-0,4-0,2 0 E / V Figure 1. Cyli voltmmogrms on opper eletrode, t 50 mv s -1 nd E l = mv, for lnk solutions with 1 M N 2 SO 4, nd: ) ph = 4, ) ph = 5.1, ) ph = 4 nd 0.2 M in sodium gluonte. Arrows indite sn diretion. -0,2 182

5 The thodi sn t 50 mv s -1 shows redution pek t round mv for the vitreous ron eletrode, ut prinipl redution pek (IIr) t round mv, preeded y smller one (Ir), for the opper eletrode. In the lter, the zin redution is followed y mssive hydrogen formtion. At lower sn rtes (Fig. 3, urve d), the pek lelled s Ir ppers well defined. Sine hydrogen evolution is importnt on opper, noise peks due to gs ules lso pper in the voltmmetri urve (see pek H in urve d of Fig. 3) nd superimpose with zin redution peks. The nodi sn t 50 mv s -1 shows prinipl pek t round mv for the vitreous ron, nd round mv for the opper eletrode (pek Io). This prinipl pek is followed y other peks whih shpe depends on the thodi limit rehed, E l, nd on the eletrode mteril. On the vitreous ron eletrode severl seondry oxidtion peks t more positive potentils re present, when E l = mv (see urve in Fig. 3), whih shift towrds the prinipl oxidtion pek or prtilly dispper when E l = mv (Fig. 2, urve ). On the opper eletrode seondry oxidtion pek (IIo), s prolongtion of the prinipl pek, is lwys present, whih eomes more importnt for more negtive vlues of E l. Eletrodeposition of zin tkes ple together with evolution of hydrogen. From the lultion of the Q + /Q - rtio (voltmmetri effiieny), where Q + nd Q - re, respetively, the oxidtion nd the redution hrges involved in the voltmmetri sns, it is oserved tht hydrogen evolves in n importnt wy, nd is more importnt on the opper eletrode (see Tle 1). At low overpotentils the hydrogen formtion is even more importnt thn the zin redution. It hs een reported in the iliogrphy [7] tht zin eletrodeposition proeeds vi metstle phses whih n present different hydrogen ontent. The presene of seondry oxidtion peks in the voltmmetri response n e ttriuted to this ft. The position nd the importne of these peks depend on severl ftors, silly the thodi limit rehed, ut lso the presene of gluonte (see next setion) nd the eletrode mteril. Tle 1 shows tht 183

6 hydrogen evolution is signifint even t low thodi limits, ut t these potentils, hydrogen n remin dsored [11] on the eletrode surfe nd trpped in the zin deposit, forming metstle hydrogented phses. At higher thodi limits, hydrogen formtion is so importnt tht evolves fr from the eletrode nd the metstle phses prtilly dispper. When the voltmmetri sn rte is redued to 10 mv s -1 (Fig. 3, urves nd d), the zin redution pek shifts to positive potentils, s is usul, while the prinipl oxidtion pek prtilly does not hnge. On the other hnd, in the nodi sn t 10 mv s -1, seondry oxidtion peks shift towrds the prinipl oxidtion pek for the vitreous ron eletrode, ut no visile hnges re seen in their position for the opper eletrode. This ehviour my e due to the evolution of the metstle phses, speilly on the vitreous ron eletrode, euse the voltmmetri experiment then lsts more time. A similr ehviour is oserved when nodi stripping experiments re performed immeditely fter potentiostti eletrodeposition with stirring. Stirring fvours hydrogen relese fr from the eletrode, hindering the formtion of the hydrogented phses, nd the seondry oxidtion peks shift towrds the prinipl pek or dispper. Io 0.4 IIo 0 Ir IIr E / V -0.8 Figure 2. Cyli voltmmogrms t 50 mv s -1 for solution 0.01 M ZnSO 4, 1 M N 2 SO 4 t ph = 4 nd E l = mv: ) vitreous ron, ) opper. Arrows indite sn diretion. 184

7 Tle 1. Q + /Q - rtios from the voltmmetri responses on vitreous ron nd on opper eletrodes, t different thodi limit potentils, E l, nd for different th onditions. [Zn 2+ ] = 0.01 M Vitreous ron [Zn 2+ ] = 0.01 M Copper [Glu]=0 [Glu]=0.2 [Glu]=0 [Glu]=0.2 ph=4 ph=5.1 ph=4 ph=5.7 ph=4 ph=4 -E l Q + /Q - Q + /Q - Q + /Q - Q + /Q - Q + /Q - Q + /Q d d 0 d IIr Ir H E/ V Figure 3. Cyli voltmmogrms for solution 0.01 M ZnSO 4, 1 M N 2 SO 4 t ph = 4 nd: ) vitreous ron, E l = mv, v = 50 mv s -1 ) vitreous ron, E l = mv, v = 10 mv s -1, ) opper, E l = mv, v = 50 mv s -1, d) opper, E l = mv, v = 10 mv s -1. Arrows indite sn diretion. Presene of gluonte Figs. 4 nd 5 present the influene of gluonte on the zin voltmmetri response. Fig. 4, when ompred with Fig. 2, shows tht on vitreous ron 185

8 (urve ), gluonte shifts slightly the zin redution to positive potentils nd tht the redution pek ppers s not well defined doule pek, insted of single pek. This ehviour is due to the omplexing tion of gluonte nions tht ompete with the omplexing tion of sulphte nions. Sine the formtion onstnt of the zin ion/gluonte omplex (log K 1 = 1.70 [15]) is lower thn tht of the zin ion/sulphte omplex (log K 1 = 2.30 [15] or 2.08 [16]), the first redution pek, Ir, n e ssigned to the gluonte-zn speies, nd the seond pek, IIr, to the sulphte-zn speies. In the nodi sn, the prinipl oxidtion pek lso ppers s doule pek. As the first oxidtion pek, Io, is situted t potentil vlue similr to tht in sene of gluonte, this pek n e ssigned to oxidtion vi sulphte nion omplextion, nd the seond pek, IIo, to the oxidtion vi gluonte nion omplextion. In the presene of gluonte, the seondry oxidtion peks t more positive potentils tend to dispper. When the voltmmetri sn rte is redued to 10 mv s -1 (Fig. 4, urve ), the zin redution pek oserved on the vitreous ron eletrode t 50 mv s -1 (Fig. 4, urve ), shifts to positive potentils ut doesn t hnging the shpe. But on the oxidtion sn, the pek Io, ssigned to oxidtion vi sulphte nion omplextion, is enhned. This ehviour my e due to kineti ftor, tht is, to higher rte of omplextion y sulphte nions of the zin ions formed in the oxidtion. At lower sn rtes, sulphte is not so depleted in the interfe lose to the eletrode nd n omplex most of the zin ions formed in the oxidtion proess. Results in Tle 1 lso show tht the Q + /Q - rtio dereses when gluonte is present in the th. It seems tht gluonte fvours hydrogen evolution nd then, s n e seen y voltmmetry, the seondry peks derese nd onsequently hydrogented metstle phses re formed with more diffiulty. On the other hnd, Fig. 4 shows tht on opper, the redution pek disppers s onsequene of n inhiitory effet of gluonte. Though zin eletrodeposition superimpose t n importnt hydrogen redution, it is seen tht on reversing the sn the voltmmetri response presents loop, with higher redution urrent, inditing lerly tht zin deposition ours. In the nodi sn roder doule 186

9 pek is formed, nd t high E l n oxidtion pek is formed t round 300 mv. This pek n e ssigned to hydrogen sine its formtion is then notiele (see Tle 1) nd its potentil orresponds to the zone of hydrogen oxidtion. Compring the voltmmetries of Fig. 5 (opper eletrode, gluonte th) with tht of the orresponding lnk solution (Fig. 1, urve ), it is seen tht in presene of zin ions the hydrogen formtion is retrded, ut lultion of the thodi nd nodi hrges indites tht the effiienies re low (Tle 1), due to the importnt hydrogen formtion. Also in the presene of gluonte, hydrogen evolves esier on opper thn on vitreous ron. At low thodi limits hydrogen formtion on opper is more importnt thn zin deposition, nd the voltmmetri urve doesn t show the hrteristi loop of deposition proess (urve in Fig. 5). Also, nd due to this ft, in the oxidtion sn smll hydrogen pek t round 300 mv is formed. Io IIo 0.2 IIr Ir E / V -1 Figure 4. Cyli voltmmogrms for solutions 0.01 M ZnSO 4, 1 M N 2 SO 4, ph = 4 nd 0.2 M sodium gluonte: ) vitreous ron, t 50 mv s -1, ) opper, t 50 mv s -1, ) vitreous ron, t 10 mv s -1. E l = mv. Arrows indite sn diretion. It seems tht in gluonte ths the zin redution on opper proeeds slower thn in non gluonte ths, nd tht the urrent vlues re lso lower. This 187

10 ehviour is opposite to tht oserved on vitreous ron, nd lso different to tht oserved for tin on vitreous ron. The differenes etween the zin ehviour nd tht of tin [14] re due to the very different vlues of the redution potentil, nd to the different vlues of gluonte nd sulphte omplextion onstnts E / V Figure 5. Cyli voltmmogrms t 50 mv s -1 for solution 0.01 M ZnSO 4, 1 M N 2 SO 4, ph = 4 nd 0.2 M sodium gluonte: ) vitreous ron, E l = mv, ) opper, E l = mv, ) opper, E l = mv. Arrows indite sn diretion. Conlusions The eletrohemil ehviour of zin from sulphte-gluonte ths is depending on the gluonte, the potentil nd the eletrode mteril. Hydrogen evolution lso proeeds with zin eletrodeposition, eing the effiieny of the proess higher on vitreous ron thn on opper. The effiieny dereses t more negtive potentils nd in the presene of gluonte, ut it is lso low t low overpotentils, where hydrogen formtion is esier thn zin redution. The zin redution tkes ple t less negtive potentils on the opper eletrode thn on the vitreous ron eletrode, speilly in sene of gluonte. On the other hnd, gluonte fvours zin eletrodeposition on vitreous ron ut retrds it on opper. 188

11 Aknowledgements This work ws supported y the CICYT MAT projet (Spin). Referenes 1. B.A. Lmping, T.J. O Keefe, Metllurg. Trnst. B, 7B (1976) A.R. Despi, M.G. Pvlovi, Eletrohim. At 27 (1982) A.C. Beshore, B.J. Flori, G. Shde, T.J. O Keefe, J. Appl. Eletrohem. 17 (1987) C. Chet, R. Wirt, J. Appl. Eletrohem. 20 (1990) A.G. Muñoz, S.B. Sidmn, J.B. Bessone, J. Appl. Eletrohem. 29 (1999) L.E.F. Teixeir, L.H. Msro, 2001 Joint Interntionl Meeting, Sn Frniso, Cliforni, strt nº E. Gómez. E. Vllés, ) Bulletin of Eletrohem. 10 (1994) 477, ) Progress in the Understnding nd Prevention of Corrosion, pg 343, Edited y J.M. Cost, A.D. Merier, The University Press, Cmridge, D.S. Bik, D.J. Fry, J. Appl. Eletrohem. 31 (2001) P.J. Sonneveld, W. Vissher, E. Brendreht, Eletrohim. At 37 (1992) L. Simnviius, A. Stkens, A. Srkis, Eletrohim. At 42 (1997) I. Epeloin, M. Ksouri, R. Wirt, J. Eletrohem. So. 122 (1975) K. Igrshi, A. Armt, S. Tguhi, Eletrohim. At 46 (2001) M. Med, Y. Nishio, 2001 Joint Interntionl Meeting, Sn Frniso, Cliforni, strt nº J. Torrent-Burgués, E. Guus, F. Snz, J. Appl. Eletrohem. 32 (2002) Stility Constnts, nº 17, Edited y The Chemil Soiety, Burlington, London, R.J. Brodd, J. Werth, in Stndrd Potentils in Aqueous Solution, pg 249, Edited y A.J. Brd, R. Prsons, J. Jordn, Mrel Dekker, NY,

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