In situ scanning tunneling microscopy study of the intergranular corrosion of copper

Martinez-Lombardia, E.; Lapeire, Linsey; Maurice, Vincent; Graeve, Iris De; Verbeken, Kim; Klein, Lorena H.; Kestens, Léo; Marcus, Philippe; Terryn, Herman

doi:10.1016/j.elecom.2014.01.007

Cited by 34 publications

(52 citation statements)

References 16 publications

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“…For the GB sites 1-4 and 8, one observes no significant variation of the depth of the GB region, which indicates that no net dissolution occurred locally and these sites are therefore classified as inert. This corrosion resistant behavior is as expected for coherent twins [7,15,37,38]. In contrast, for the GB sites 5-7 and 9, the bottom of the GB region became deeper after 4 CVs, indicating that copper was irreversibly dissolved and that these sites are reactive.…”

Section: Corrosion Behavior Of 3 Grain Boundariessupporting

confidence: 79%

Nanoscale Intergranular Corrosion and Relation with Grain Boundary Character as Studied In Situ on Copper

Bettayeb

Maurice

Klein

et al. 2018

J. Electrochem. Soc.

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The initiation of intergranular corrosion at various types of grain boundaries (GBs) was studied at the nanometer scale on microcrystalline copper in 1 mM HCl aqueous solution. In situ Electrochemical Scanning Tunneling Microscopy (ECSTM) and Electron Back-Scatter Diffraction analysis of the same local microstructural region were combined using an innovative methodology including micro marking performed with the STM tip. The results demonstrate that electrochemically-induced intergranular dissolution, at the surface termination of GBs, is dependent on the grain boundary character. It is found that random high angle boundaries as well as 9 coincidence site lattice (CSL) boundaries are susceptible to nanoscale initiation of intergranular corrosion while for 3 CSL boundaries the behavior is dependent on the deviation angle of the GB plane from the exact orientation. For the 3 twins, a transition from resistance to susceptibility occurs between 1° and 1.7° of deviation as a result of the increase of the density of steps (i.e. misorientation dislocations) in the coincidence boundary plane. The work emphasizes the precision needed in the design of the grain boundary network in applications where intergranular corrosion or its initiation must be controlled at the nanoscale.

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Section: Corrosion Behavior Of 3 Grain Boundariessupporting

confidence: 79%

Nanoscale Intergranular Corrosion and Relation with Grain Boundary Character as Studied In Situ on Copper

Bettayeb

Maurice

Klein

et al. 2018

J. Electrochem. Soc.

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show abstract

“…These observations are consistent with published studies showing similar etching in acidic solutions. 35 Figure 7(e) shows a series of Raman spectra recorded at various locations on the corroded surface. The peaks at 525 cm −1 , 625 cm −1 , 147 cm −1 , and the faint peak at 220 cm −1 indicate the presence of Cu 2 O.…”

Section: Resultsmentioning

confidence: 99%

The Effects of Cathodic Reagent Concentration and Small Solution Volumes on the Corrosion of Copper in Dilute Nitric Acid Solutions

et al. 2017

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The exposure conditions experienced by copper-coated highlevel nuclear waste containers in a deep geologic repository will evolve with time. An early exposure period involving the gamma irradiation of aerated humid vapor could lead to the formation of nitric acid condensed in limited volumes of water on the container surface. The evolution of the corrosion processes under these conditions have been studied using pH measurements in limited volumes of water containing various concentrations of nitric acid. The extent and morphology of corrosion was examined using scanning electron microscopy on surfaces and on focused ion beam cut cross sections. The composition of corrosion products was determined by energy dispersive x-ray analyses and Raman spectroscopy. In the absence of dissolved oxygen only minor corrosion was observed with the reduction of nitric acid inhibited by the formation of either chemisorbed nitrate and nitrite species or the formation of a thin cuprite (Cu 2 O) layer. When the solution was aerated, both oxygen and nitric acid acted as cathodic reagents. After extensive exposure periods corrosion was stifled by the formation of corrosion product deposits of Cu 2 O, CuO (tenorite), and Cu 2 NO 3 (OH) 3 (rouaite).

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“…EBSD revealed a nearly random texture of the grains with a ∑3 CSL boundaries length fraction of 66%. The remaining 34% corresponded to random boundaries for the most part [22,23]. Surface preparation was performed by mechanical polishing with diamond spray down to a final grade of 0.25 μm.…”

Section: Methodsmentioning

confidence: 99%

“…This is due to the difficulty 3 of applying analytical methods sensitive to the electrochemically-induced local alterations of the topmost surface. Recently, ECSTM (Electro-Chemical Scanning Tunneling Microscopy) has been applied to microcrystalline copper to investigate in situ the local corrosion resistance at the surface termination of grain boundaries in metals [22][23][24][25][26]. It was found that dissolution in the active state, i.e.…”

Section: Introductionmentioning

confidence: 99%

Combined in situ microstructural study of the relationships between local grain boundary structure and passivation on microcrystalline copper

Bettayeb

Maurice

Klein

et al. 2019

Electrochimica Acta

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In situ Electro-Chemical Scanning Tunneling Microscopy (ECSTM) and Electron Back-Scatter Diffraction analysis of the same local microstructural region were combined to study the relationships between grain boundary (GB) type and structure and passivation on microcrystalline copper in 0.1 M NaOH aqueous solution. The results show that, for high angle random boundaries, passivation in the Cu(I) oxidation range is characterized by a decrease of the depth of GB edge region due to the formation of a passive film locally thicker than on the adjacent grains and thus to anodic oxidation being locally less efficient since it consumes more copper at the grain boundaries. For 3 CSL boundaries, the Cu(I) passivation efficiency was observed to be dependent on the local structure of the boundaries. A transition from more to less efficient passivation was observed for a deviation angle of 0.4-0.5° of the {111} GB plane with respect to the perfect geometry of an ideal coherent twin boundary. This transition would result from the effect on the local anodic oxidation properties of an increased density of misfit dislocations accommodating the increased deviation of the boundary plane from the exact CSL plane.

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In situ scanning tunneling microscopy study of the intergranular corrosion of copper

Cited by 34 publications

References 16 publications

Nanoscale Intergranular Corrosion and Relation with Grain Boundary Character as Studied In Situ on Copper

Nanoscale Intergranular Corrosion and Relation with Grain Boundary Character as Studied In Situ on Copper

The Effects of Cathodic Reagent Concentration and Small Solution Volumes on the Corrosion of Copper in Dilute Nitric Acid Solutions

Combined in situ microstructural study of the relationships between local grain boundary structure and passivation on microcrystalline copper

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