Growth and Degradation of an Anodic Oxide Film on Titanium in Sulphuric Acid Observed by Ellipso-microscopy

Fushimi, Koji; Kurauchi, K.; Yamamoto, Yoshihiko; Nakanishi, Takayuki; Hasegawa, Yasuchika; Ohtsuka, Toshiaki

doi:10.1016/j.electacta.2014.08.082

Cited by 19 publications

(25 citation statements)

References 31 publications

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“…The quantitative distribution in thickness and optical property is strongly dependent on crystallographic orientation of the substrate as well as the potential applied. 39 The oxide breakdown taking place the solution containing bromide ions 39 and photo-electrochemical degradation of oxide film on titanium 40 were also observed by using the in-situ ellipso-microscopy. It is very interested in evaluation of the surface heterogeneity under the in-situ condition and an instant initiation of breakdown on the passive oxide film can be detected in future.…”

Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

“…39 During the potential sweep to the positive direction, the PCSA optical configuration was kept constant which was initially controlled in the extinction state at the OCP. When the oxide growth occurs with the potential increase, the brightness gradually increases.…”

Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

“…Schematic diagram of the set-up of ellipso-microscopy. 39 (a) specimen, (b) counter electrode, (c) reference electrode, (d) electrolyte solution, (e) laser, (f ) beam splitter, (g) light intensity monitor, (h) depolarizer, (i) polarizer, P, (j) compensator, C, (k) analyzer, A, (l) CMOS camera, (m) macro-lens for ellipso-microscopy, (n) CMOS camera for specimen observation, (o) macro-lens for specimen observation, (p) potentiostat and function generator, (q) PC. The image of ellipso-microscopy on the camera from OCP to 8 V. The configuration of PSCA arrangement was fixed at an extinction state under the initial OCP condition.…”

Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

“…The image of ellipso-microscopy on the camera from OCP to 8 V. The configuration of PSCA arrangement was fixed at an extinction state under the initial OCP condition. 39 Electrochemistry, 84(11), 826-832 (2016)…”

Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

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Optical Characterization of Passive Oxides on Metals

Ohtsuka

Fushimi

2016

Electrochemistry

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In-situ optical detection of the passive oxide films on iron and titanium was reviewed. The optical techniques such as ellipsometry (i.e., reflection of polarized light), Raman spectroscopy, and potential modulation reflectance (PMR) have been successfully applied to the detection in thickness, composition, and semiconducting property, respectively, of the thin passive oxides under the in-situ condition. The growth mechanism of the passive oxide has been discussed from the precise measurement of thickness as a function of potential and time by a threeparameter ellipsometry. From the in-situ Raman spectra, the composition of the passive oxide has been estimated to be Fe 3 O 4 -γ-Fe 2 O 3 for iron and anatase TiO 2 for titanium. From PMR, the Mott-Schottky type plot could be drawn in the passive oxide on iron, which indicates that the formation of the space charge layer can be optically seen. From the PMR spectra, one has evaluated light-absorption edge that may correspond to a band-gap energy between the valence and conduction band.© The Electrochemical Society of Japan, All rights reserved.Keywords : Passive Oxide Film, Ellipsometry, Raman Spectroscopy, Ellipso-microscopy Corrosion Protection and Passivation of MetalsMetallic materials are widely used for construction of infrastructure such as bridge, building, industrial plant etc. and transport machine such as automobile, ship, train, airplane etc. For using the metallic materials for a long period of time, suitable protection against corrosion has been required. When the structures are used in atmospheric environment that includes 21% oxygen and small amount of water vapor, they suffers considerable damage because of corrosion induced by the oxygen and water vapor. The water vapor adsorbs on the metal surface with contaminant such as dust, fine particle, and air-borne salt to provide liquid water layer. The water layer in which various compounds dissolve acts on the metal surface as an electrochemical reaction site in which corrosion reactions occur; an anodic oxidation reaction of the metal is coupled with a cathodic reduction reaction of oxygen dissolving into the water layer.The structures are also often used in sea, lake, marsh, and moist soil.Since the interface at metal surface/surrounding water also acts as a reaction site, the corrosion of the structures takes place similarly as in the atmospheric environment. Since the metallic corrosion continues to develop in the atmospheric condition on the earth, we must introduce corrosionprotection treatment to maintain the structure for a long period. We have applied several techniques to the corrosion protection.(i) Cathodic protection: The potential of the structural metal is shifted to the negative direction to lower the corrosion rate. (ii) Anodic protection or passivation: The potential of the metals is shifted to the positive direction in the passive potential region in which the corrosion rate is negligibly small. (iii) Inhibition of contact to the surrounding environment: The cover of paint o...

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Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

Section: Heterogeneity Of Passive Oxide By Ellipso-microscopymentioning

confidence: 99%

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Optical Characterization of Passive Oxides on Metals

Ohtsuka

Fushimi

2016

Electrochemistry

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“…They suggested that UV-light irradiation resulted in occurrence of non-uniform corrosion. Recently, the authors developed an electrochemical ellipso-microscope to monitor an electrode surface and reported non-uniform change of anodic oxide film on titanium 3) . Degradation of oxide film due to bromo-oxide formation as well as growth of the film was observed as a change in optical condition of the ellipso-microscope.…”

Section: Introductionmentioning

confidence: 99%

Ellipso-Microscopic Observation of Titanium Surface under UV-Light Irradiation

Fushimi¹,

Kurauchi²,

Nakanishi³

et al. 2016

Corrosion Science and Technology

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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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Growth and Degradation of an Anodic Oxide Film on Titanium in Sulphuric Acid Observed by Ellipso-microscopy

Cited by 19 publications

References 31 publications

Optical Characterization of Passive Oxides on Metals

Optical Characterization of Passive Oxides on Metals

Ellipso-Microscopic Observation of Titanium Surface under UV-Light Irradiation

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

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