Rotating ring-disk electrochemical quartz crystal microbalance: a new tool for in situ studies of oxide film formation

Vergé, M.-G.; Mettraux, P.; Olsson, Claes; Landolt, D.

doi:10.1016/j.jelechem.2003.11.047

Cited by 12 publications

(14 citation statements)

References 29 publications

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“…As compared to other valve metals Ti shows several significant differences regarding its anodic oxidation behavior mainly due to the distinct semiconducting character of the formed anodic oxide layer. The n‐type semiconducting properties of anodic titanium oxides are enabling electronic currents during anodization leading to side reactions during anodization like oxygen evolution …”

Section: Figurementioning

confidence: 99%

“…The measured current can be generated by different electrochemical processes on titanium such as oxide growth, metal dissolution or oxygen evolution. Among the scientific reports dealing with corrosion phenomena during anodization, most are reporting the Ti concentration in the electrolyte after oxide growth as measured by spectroscopic methods like AAS or are relying on indirect measurements like using an electrochemical quartz crystal microbalance (ECQM) or ellipsometry …”

Section: Figurementioning

confidence: 99%

“…This significant current increase is a result of the oxygen evolution which becomes possible in this potential range due to electronic conduction through the oxide . The oxygen evolution was directly observed by Landolt et al . using a special rotating ring‐disc electrode (RRDE) setup.…”

Section: Figurementioning

confidence: 99%

“…Landolt et al. also performed electrochemical quartz crystal microbalance experiments during anodization of a sputtered thin film in diluted sulfuric acid. During the forward scan they first found a mass increase of the titanium electrode indicating the growth of an oxide film.…”

Section: Figurementioning

confidence: 99%

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In Situ Monitoring of Ionic Metal Dissolution During Anodization of Titanium and Quantification of Parallel Electronic Oxygen Evolution

Kollender

Hassel

2017

ChemElectroChem

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This study reports an in situ investigation of the metal dissolution during anodization of titanium. A combination of an electrochemical flow cell that is directly coupled to an ICP‐MS was used for the investigation. The oxide film was grown through potentiodynamic anodization (CV with 10 mV s−1) between 0 and 8 V. A rather constant dissolution rate of approximately 1.5 ng s−1 cm−2 was observed during the entire oxide formation although the current, as measured by the potentiostat, increased from 58 μA cm−2 (1 V) up to 290 μA cm−2 (8 V). Controversially, the dissolution rate was not affected by the additional electronic currents, which become relevant for potentials higher than 3.5 V. The metal dissolution is triggered by the ionic species (Ti4+ and O2−) crossing the oxide layer (ionic currents) under the applied high‐field conditions. No reduction of the oxide during the reverse scan could be observed. The fraction of charge carriers used for metal dissolution stayed rather constant (ca. 21 %) up 3.5 V, and then continuously decreased to 4 % for the highest applied anodization potential (8.0 V), reflecting the increased oxygen evolution rate at a rather constant dissolution rate.

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Section: Figurementioning

confidence: 99%

Section: Figurementioning

confidence: 99%

Section: Figurementioning

confidence: 99%

Section: Figurementioning

confidence: 99%

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In Situ Monitoring of Ionic Metal Dissolution During Anodization of Titanium and Quantification of Parallel Electronic Oxygen Evolution

Kollender

Hassel

2017

ChemElectroChem

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“…ECQCM has existed for many years (33)(34)(35)(36)(37)(38)(39)(40)(41), even as commercial instruments, but not ECQCM-D. This combination is valuable for adsorption studies under the influence of external fields (34) and/or when one wants to change in situ the oxide layer thickness (35)(36)(37)(38)(39)(40)(41). Fleming et al (42) have employed ECQCM-D to study the adsorption of azurin on a gold electrode modified with an alkanethiol self-assembled monolayer.…”

Section: Introductionmentioning

confidence: 99%

In Situ Control of the Oxide Layer on Thermally Evaporated Titanium and Lysozyme Adsorption by Means of Electrochemical Quartz Crystal Microbalance with Dissipation

Keere

Svedhem

Högberg

et al. 2008

ACS Appl. Mater. Interfaces

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Electrochemical (EC) quartz crystal microbalance with dissipation monitoring (ECQCM-D) is a new and powerful technique for the in situ study of adsorption phenomena, e.g., as a function of the potential of the substrate. When titanium (Ti) is employed as the substrate, its oxidation behavior needs to be taken into account. Ti is always covered with a native oxide layer that can grow by, e.g., thermal oxidation or under anodic polarization. For biomolecular adsorption studies on oxidized Ti under applied potential, a stable oxide layer is desired in order to be able to distinguish the adsorption phenomena and the oxide growth. Therefore, the oxidation of thermally evaporated Ti films was investigated in phosphate-buffered saline by means of ECQCM-D, using a specially designed EC flow cell. Upon stepping the potential applied to Ti up to 2.6 V vs standard hydrogen electrode (SHE), a fast increase of the mass was observed initially for each potential step, evolving slowly to an asymptotic mass change after several hours. The oxide layer thickness increased as a quasi-linear function of the oxidation potential for potentials up to 1.8 V vs SHE. The growth rate of the oxide was around 2.5-3 nm/V. No changes in the dissipation shift were observed for potentials up to 1.8 V vs SHE. The composition of the oxide layer was analyzed by X-ray photoelectron spectroscopy (XPS). It was mainly composed of TiO(2), with a small percentage of suboxides (TiO and Ti(2)O(3)) primarily at the inner metal/oxide interface. The amount of TiO(2) increased, and that of TiO and Ti(2)O(3) decreased, with increasing oxidation potential. For each oxidation potential, the calculated thickness obtained from ECQCM-D correlated well with the thickness obtained by XPS depth profiling. A procedure to prepare Ti samples with a stable oxide layer was successfully established for investigations on the influence of an electric field on the adsorption of biomolecules. As such, the effect of an applied potential on the adsorption behavior of lysozyme on oxidized Ti was investigated. It was observed that the adsorption of lysozyme on oxidized Ti was not influenced by the applied potential.

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Electrochemical Quartz Crystal Microbalance

Ispas¹,

Bund²

2014

Encyclopedia of Applied Electrochemistry

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Rotating ring-disk electrochemical quartz crystal microbalance: a new tool for in situ studies of oxide film formation

Cited by 12 publications

References 29 publications

In Situ Monitoring of Ionic Metal Dissolution During Anodization of Titanium and Quantification of Parallel Electronic Oxygen Evolution

In Situ Monitoring of Ionic Metal Dissolution During Anodization of Titanium and Quantification of Parallel Electronic Oxygen Evolution

In Situ Control of the Oxide Layer on Thermally Evaporated Titanium and Lysozyme Adsorption by Means of Electrochemical Quartz Crystal Microbalance with Dissipation

Electrochemical Quartz Crystal Microbalance

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