Abstract
Palladium nanoparticles and nanowires electrochemically deposited onto a carbon surface were studied using cyclic voltammetry, impedance spectroscopy and atomic force microscopy. The ex situ and in situ atomic force microscopy (AFM) topographic images showed that nanoparticles and nanowires of palladium were preferentially electrodeposited to surface defects on the highly oriented pyrolytic graphite surface and enabled the determination of the Pd nanostructure dimensions on the order of 50–150 nm. The palladium nanoparticles and nanowires electrochemically deposited onto a glassy carbon surface behave differently with respect to the pH of the electrolyte buffer solution. In acid or mild acid solutions under applied negative potential, hydrogen can be adsorbed/absorbed onto/into the palladium lattice. By controlling the applied negative potential, different quantities of hydrogen can be incorporated, and this process was followed, analysing the oxidation peak of hydrogen. It is also shown that the growth of the Pd oxide layer begins at negative potentials with the formation of a pre-monolayer oxide film, at a potential well before the hydrogen evolution region. At positive potentials, Pd(0) nanoparticles undergo oxidation, and the formation of a mixed oxide layer was observed, which can act as nucleation points for Pd metal growth, increasing the metal electrode surface coverage. Depending on thickness and composition, this oxide layer can be reversibly reduced. AFM images confirmed that the PdO and PdO2 oxides formed on the surface may act as nucleation points for Pd metal growth, increasing the metal electrode surface coverage.
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Harrison BS, Atala A (2007) Biomaterials 28:344
He X, Wu F, Zheng M (2006) DOI 10.1016/j.diamond.2006.06.011
Kohli P, Wirtz M, Martin CR (2004) Electroanalysis 16:9
Welch CM, Compton RG (2006) Anal Bioanal Chem 384:601
Katz E, Willner I, Wang J (2004) Electroanalysis 16:19
Simm AO, Ward-Jones S, Banks CE, Compton RG (2005) Anal Sci 21:667
Raj CR, Okajima T, Ohsaka T (2003) J Electroanal Chem 543:127
Liu H, Favier F, Ng K, Zach MP, Penner RM (2001) Electrochim Acta 47:671
Penner RM (2002) J Phys Chem B 106:3339
Walter EC, Murray BJ, Favier F, Kaltenpoth G, Grunze, M, Penner RM (2002) J Phys Chem B 106:11407
Kawde A-N, Wang J (2004) Electroanalysis 16:101
Willner B, Katz E, Willner I (2006) Curr Opin Biotech DOI 10.1016/j.copbio.2006.10.008
Martínez-Sánchez R, Reyes-Gasga J, Caudillo R, García-Gutierrez DI, Márquez-Lucero A, Estrada-Guel I, Mendoza-Ruiz DC, José Yacaman M (2006) J Alloy Compd DOI 10.1016/j.jallcom.2006.08.051
Dávila-Martínez RE, Cueto LF, Sánchez EM (2006) Surf Sci 600:3427
Ng KH, Liu H, Penner RM (2000) Langmuir 16:4016
Mayrhofer KJJ, Arenz M, Blizanac BB, Stamenkovic V, Ross PN, Markovic NM (2005) Electrochim Acta 50:5144
Zoval JV, Lee J, Gorer S, Penner RM (1998) J Phys Chem B 102:1166
You T, Niwa O, Chen Z, Hayashi K, Tomita M, Hirono S (2003) Anal Chem 75:5191
Xu C, Wu G, Liu Z, Wu D, Meek TT, Han Q (2004) Mater Res Bull 39:1499
Male KB, Hrapovic S, Liu Y, Wang D, Luong JHT (2004) Anal Chim Acta 516:35
Sun YP, Li XQ, Cao J, Zhang WX, Wang HP (2006) Adv Colloid Interface Sci 120:47
Charles E, Sykes H, Fernandez-Torres LC, Nanayakkara SU, Mantooth BA, Nevin RM, Weiss PS (2005) Proc Natl Acad Sci USA 102:17907
Burke LD, Casey JK (1993) J Electrochem Soc 140:1284
Burke LD, Casey JK (1993) J Electrochem Soc 140:1292
Burke LD, Casey JK (1993) J Appl Electrochem 23:573
Bolzán AE (1995) J Electroanal Chem 380:127
Chierchie T, Mayer C, Lorentz WJ (1982) J Electroanal Chem 135:211
Gossner K, Mizera E (1981) J Electroanal Chem 125:347
Baldauf M, Kolb DM (1993) Electrochim Acta 38:2145
Naohara H, Ye S, Uosaki K (1998) J Phys Chem B 102:4366
Lubert K-H, Guttman M, Beyer L (1999) J Electroanal Chem 462:174
Lubert K-H, Guttman M, Beyer L, Kalcher K (2001) Electrochem Commun 3:102
Li F, Zhang B, Dong S, Wang E (1997) Electrochim Acta 42:2563
Pattabiraman R (1997) Appl Catal A Gen 153:9
Batchelor-McAuley C, Banks CE, Simm AO, Jones TGJ, Compton RG (2006) Chem Phys Chem 7:1081
Fournée V, Barrow JA, Shimoda M, Ross AR, Lograsso TA, Thiel PA, Tsao AP (2003) Surf Sci 541:147
Ji X, Banks CE, Xi W, Wilkins SJ, Compton RG (2006) J Phys Chem B 110:22306
Atshabar MZ, Banerji D, Singamaneni S, Bliznuyuk V (2004) Nanotechnology 15:374
Handbook of chemistry and physics http://www.hbcpnetbase.com/
Czrewinski A, Marassi R, Zamponi S (1991) J Electroanal Chem 316:211
Burke LD, Nagle LC (1999) J Electroanal Chem 461:52
Burke LD, Casey JK (1992) Electrochim Acta 37:1817
Markovic NM, Sarrat ST, Gasteiger HA, Ross PN (1996) J Chem Soc Faraday Trans 92:3719
Tani T (1989) Phys Today 36:36
Bagotzky VS, Tarasevich MR (1979) J Electroanal Chem 101:1
Kim KS, Gossmann AF, Winograd N (1974) Anal Chem 46:197
Acknowledgements
Financial support from Fundação para a Ciência e Tecnologia (FCT), Post-Doctoral Grants SFRH/BPD/18824/2004 (V.C. Diculescu), SFRH/BPD/27087/2006 (A.M. Chiorcea-Paquim), Ph.D. Grant SFRH/BD/18914/2004 (O. Corduneanu), POCI 2010 (co-financed by the European Community Fund FEDER), ICEMS (Research Unit 103), is gratefully acknowledged.
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Dedicated to Professor Dr. Algirdas Vaskelis on the occasion of his 70th birthday.
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Diculescu, V.C., Chiorcea-Paquim, AM., Corduneanu, O. et al. Palladium nanoparticles and nanowires deposited electrochemically: AFM and electrochemical characterization. J Solid State Electrochem 11, 887–898 (2007). https://doi.org/10.1007/s10008-007-0275-7
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DOI: https://doi.org/10.1007/s10008-007-0275-7