Anodic Oxidation of Copper in Alkaline Solutions: I . Nucleation and Growth of Cupric Hydroxide Films

Shoesmith, D.W.; Rummery, T. E.; Owen, Derrek G.; Lee, W.

doi:10.1149/1.2132934

Cited by 104 publications

(71 citation statements)

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“…Electrochemical anodization processes were known to form a porous Cu 2 O layer at first, and then Cu(OH) 2 or CuO films on it. 27,28 Bouillon et al found that only CuO was observed at low current density (< 0.5 mA cm -2 ), and Cu(OH)2 was dominant at above 0.8 mA cm -2 . 29 In the light of these previous reports, we can interpret our results as followings: 1) at 0.1 mA cm -2 , Cu foil is covered with only the porous Cu2O particles because of a small current density for the growth of Cu(OH)2 or CuO films; 2) sheet-shape CuO mainly grows at 0.5 mA cm -2 ; 3) the growth of 1D Cu(OH)2 nanostructures, competing with the formation of CuO, become more favorable with increasing a higher current density between 1 -2 mA cm -2 .…”

Section: The Concentration Of Nucleophile Ohmentioning

confidence: 99%

“…7 Various copper compound nanostructures, including nanotubes, nanowires, whiskers and nanosheets, have been grown directly by the chemical oxidation of copper foil in alkaline aqueous solutions with an oxidant additive [8][9][10][11] or by the electrochemical anodization in an alkaline solutions. 12 In particular, Xu and co-workers successfully prepared Cu(OH)2 nanowire and nanotube arrays on a copper substrate via the electrochemical route using an electrolyte solution of KOH. 13 This electrochemical method has an advantage over other methods in that the shape and atomic compositions of final copper compound films can be controlled by means of modulating the potential, reaction time, and the integrated charge passed through the cell.…”

Section: Introductionmentioning

confidence: 99%

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Wire-like Bundle Arrays of Copper Hydroxide Prepared by the Electrochemical Anodization of Cu Foil

La¹,

Park²,

Choi

et al. 2010

Bulletin of the Korean Chemical Society

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Nanostructured copper compounds were grown by electrochemical anodization of copper foil in aqueous NaOH under varying conditions including electrolyte concentration, reaction temperature, current density, and reaction time. Their morphology and atomic composition were investigated by using SEM, TEM, XRD, EDS and XPS. At the con-), wire-like orthorhombic Cu(OH)2 nanobundles with an average width of 100 -300 nm and length of 10 µm were synthesized with the preferential [100] growth direction. Furthermore, when the concentration decreased to 0.5 M NaOH, the 1D nanobundle structure became narrower and longer without any change in compositions or crystalline structure. Side reaction pathways appeared to compete with the 1D nanostructure formation channels: the formation of CuO nanoleaves at 50 o C via the sequential dehydration of Cu(OH)2, CuO/Cu2O aggregates in 4 M NaOH, and Cu2O nanoparticles and CuO nanosheets at lower current density.

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Section: The Concentration Of Nucleophile Ohmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Wire-like Bundle Arrays of Copper Hydroxide Prepared by the Electrochemical Anodization of Cu Foil

La¹,

Park²,

Choi

et al. 2010

Bulletin of the Korean Chemical Society

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“…L'ttape lente est la diffusion des ions (CuBr;;,), et la vitesse de la rtaction forrnCe par les Ctapes [4] et [5] est donnte par la prernikre loi de Fick, dont la forrne sirnplifite est: [6] (CuBrTi ,I, [7] v = XFD Pour sa part, I'utilisation de l'tlectrode ii disque tournant permet d'tcrire l'tquation de Levich (1 1):…”

Section: Quantite' De Bromure Cuivreux Accumulce Durantunclassified

“…La substitution de 6 dans la relation [7] donne: ou X, la charge de ou des espkces qui diffusent, est comprise entre I et 2; v, la viscositt cintrnatique, est voisine de 0,96 x lo-' cm' s-' (12); Dc,Br;;,r est le coefficient de diffusion de l'espkce CuBr,, ~u~r iou des deux espkces a la fois, selon la valeur de X; (CuBr;,,), est la concentration en cuivre a la surface de 1'Clectrode alors que o est la vitesse de rotation de l'tlectrode en radians par seconde.…”

Section: Quantite' De Bromure Cuivreux Accumulce Durantunclassified

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Etude de la dissolution du bromure cuivreux formé sur le cuivre

Brossard¹

1984

Can. J. Chem.

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1 12 (1984).La dissolution du bromure cuivreux, form6 par oxydation Clectrochimique du cuivre immergC en solution aqueuse de NaBr, a CtC CtudiCe. La concentration en NaBr a Ct C variCe de 0,l M a 1,2 M alors que le pH Ctait de 4. Le produit de corrosion accumulC sur 1'Clectrode est constituC de cristaux de CuBr y. La prtsence de ce composC contribue a I'enrichissement local de la solution en cuivre dissous pr6s de I'Clectrode. Cet enrichissement se traduit par une tension d7Clectrode en circuit ouvert bien caractkristique. Elle est Cgale a environ -149 mV (ECS) sur une Clectrode en position stationnaire immergte dans une solution 0,2 M NaBr. La dissolution complete du CuBr coincide, pour sa part, a une chute rapide de la tension. Cette chute de tension a permis de dCfinir le temps de transition T a partir duquel la vitesse de dissolution du CuBr a Ct C calculte. Par exemple, la vitesse de dissolution est de 0,074 f 0,003 mA cm-' en courant tquivalent pour une Clectrode en position stationnaire en prCsence d'une solution 0,2 M NaBr non agitCe. Elle est aussi constante jusqu'i la disparition complkte du composC. Par ailleurs, I'utilisation de I'Clectrode a disque tournant a mis en evidence que la dissolution est entierement dominee par la diffusion des ions en phase liquide. Les rCsultats experimentaux sont compatibles avec la presence simultanCe du CuBr, et du ~u~r tcomme especes diffusantes. Enfin, les courbes de polarisation potentiodynamiques montrent deux vagues d'oxydation. Une portion non nkgligeable du courant de dissolution, sinon la quasi-totalitt, se traduit par la formation de CuBr sur I'tlectrode qui est le seul produit de corrosion prCsent.ROBERT-LOUIS BROSSARD. Can. J . Chem. 62, 1 1 12 (1984).' The dissolution of cuprous bromide, formed by the electrochemical oxidation of copper immersed in aqueous NaBr, has been studied. NaBr concentration was varied between 0. I and 1.2 M at pH 4. The corrosion product accumulating on the electrode is crystalline y-CuBr. The presence of this material contributes to the local enrichment of dissolved copper close to the electrode. This enrichment leads to a characteristic electrode voltage in open circuit, which is about -149 mV (ECS) at a stationary electrode immersed in a solution of 0.2 M NaBr. The complete dissolution of CuBr coincides with a rapid fall in voltage which permits the definition of the transition time T from which the speed of CuBr dissolution has been calculated. For example, the speed of dissolution is 0.074 2 0.003 mA cm-' in a current equivalent for a stationary electrode in the presence of a non-stirred solution of 0.2 M NaBr. This is constant until the complete disappearance of the CuBr. On the other hand, use of a rotating disc electrode demonstrates that the dissolution is entirely dominated by the diffusion of ions in the liquid phase. The experimental results are compatible with the simultaneous presence of CuBr, and CUB^:-as diffusing species.Finally, the potentiodynamic polarization curves show two oxidation waves. A non-negligible por...

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Multi-method Analysis of the Metal/Electrolyte Interface: Scanning Force Microscopy (SFM), Quartz Microbalance Measurements (QMB), Fourier Transform Infrared Spectroscopy (FTIR) and Grazing Incidence X-ray Diffractometry (GIXD) at a Polycrystalline Copper Electrode

Kautek

Geuss

Sahre

et al. 1997

Surf. Interface Anal.

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The successful application of various in situ and ex situ analytical techniques has been demonstrated at the buried interface between a metal and an electrolyte. Scanning force microscopy (SFM), electrochemical quartz microbalance measurements (EQMB), grazing incidence x‐ray diffractometry (GIXD), Fourier transform infrared spectroscopy (FTIR) in the specular reflection absorption mode and electrochemical charge measurements proved complementary in the characterization of a polycrystalline copper electrode in alkaline 0.1 M sulphate, perchlorate, fluoride and chloride electrolyte contact at pH 12. The surface exhibited a mixture of Cu(111) and Cu(200) grains of the order of 100 nm. Repeated potential scanning in the double layer and passive oxide region, between ‐1.4 and +0.1 VMSE, resulted in a complete reorganization of the surface morphology but no detectable corrosion. The electrochemical exchange of H2O and OH− between the electrolyte and the oxide film took place reversibly in accordance with a solid‐state growth mechanism. The copper atoms were redeposited at crystallographically preferred sites, generating comparatively homogeneously oriented, narrow Cu(111)‐edged grain ridges of length 200 nm. In the Cu(I) potential range, the formation of several monolayers of amorphous Cu2O could be confirmed. Only after extended time periods in the Cu(II) oxide potential region, Cu2O recrystallized to a (111) phase accompanied by Cu2O(200) and Cu2O(110). In this region, one observed the formation of amorphous Cu(OH)2 concurrent with further growth of Cu2O. Strong CuOH IR stretching bands excluded the existence of CuO. At corrosive potentials of +0.25 VMSE, high anodic currents and substantial mass losses led to an electropolished surface with isolated features of <300 nm width and <70 nm height.© 1997 John Wiley & Sons, Ltd.

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Anodic Oxidation of Copper in Alkaline Solutions: I . Nucleation and Growth of Cupric Hydroxide Films

Cited by 104 publications

References 30 publications

Wire-like Bundle Arrays of Copper Hydroxide Prepared by the Electrochemical Anodization of Cu Foil

Wire-like Bundle Arrays of Copper Hydroxide Prepared by the Electrochemical Anodization of Cu Foil

Etude de la dissolution du bromure cuivreux formé sur le cuivre

Multi-method Analysis of the Metal/Electrolyte Interface: Scanning Force Microscopy (SFM), Quartz Microbalance Measurements (QMB), Fourier Transform Infrared Spectroscopy (FTIR) and Grazing Incidence X-ray Diffractometry (GIXD) at a Polycrystalline Copper Electrode

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