High Speed Atomic Force Microscope Observation of Polyethylene Glycol Adsorption on Au(100)

Esaki, Rei; Yasuda, Yasuhiko; Kotani, Norito; Matsushima, Hisayoshi; Ueda, Mikito

doi:10.1149/1945-7111/ac876c

Cited by 3 publications

(3 citation statements)

References 24 publications

(34 reference statements)

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“…In other words, the gauche conformations decrease to a larger extent as compared to the trans conformations, indicating that the compact mound-like adsorption structure of PEG-Cl – could be loosened with decreasing potential. In fact, high-speed EC-AFM observation for PEG-Cl – adsorption on Au(100) revealed a structural change from spheres to large irregular clusters with negative-going potential over a certain range . Besides, the peaks at 2877, 1465, 1254, and 850 cm –1 related to −CH 2 – of PEG clearly decrease at potentials negative of −0.65 V, suggesting that PEG mounds turn loose and even partially desorb at a critical potential .…”

Section: Resultsmentioning

confidence: 98%

“…In fact, high-speed EC-AFM observation for PEG-Cl − adsorption on Au(100) revealed a structural change from spheres to large irregular clusters with negativegoing potential over a certain range. 51 Besides, the peaks at 2877, 1465, 1254, and 850 cm −1 related to −CH 2 − of PEG clearly decrease at potentials negative of −0.65 V, suggesting that PEG mounds turn loose and even partially desorb at a critical potential. 13 Moreover, as shown in Figure 5a, the downward peak at ca.…”

Section: Mound Model For Peg-clmentioning

confidence: 94%

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Revisiting the Polyethylene Glycol-Chloride Adsorption Structure on Cu Electrode in Sulfuric Acid Solution by Wide-Frequency ATR-SEIRAS

Wu,

Mao,

Jiang

et al. 2023

J. Phys. Chem. C

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Polyethylene glycol (PEG) is a typical suppressor in the presence of chloride anions for Cu interconnect electroplating in the field of microelectronics manufacture, yet its adsorption structure and its correlation with the inhibition effect remain controversial and unclear. In this work, wide-frequency attenuated total reflection surface-enhanced infrared absorption spectroscopy (ATR-SEIRAS) is utilized to clarify the interfacial adsorption structure of PEG with Cl– on a Cu electrode, providing direct molecular-level evidence for the inhibition effect. Time-resolved spectroscopic results show that the OC–CO subunit of PEG transforms from trans to gauche conformation with the addition of Cl– in a way favoring the hydrocarbon sections of PEG to lean toward the Cl–-covered Cu surface, as demonstrated by the evolution of characteristic peaks at 1134, 1090, and 848 cm–1 as well as that of interfacial water stretching vibration bands (ca. 3400–3650 cm–1). Moreover, a comparison of spectra for adsorbed PEG and dissolved PEG shows that more OC–CO and CC-OC gauche conformations are present in the former, in favor of PEG chain coiling to form mounds on the Cl–-covered Cu electrode. The steric hindrance of as-formed PEG mounds may account for the strong interfacial inhibition effect of the PEG-Cl– adstructure, as supported by the electrochemical quartz crystal microbalance (EQCM) measurement. A series of potential-dependent ATR-SEIRAS spectra reveal that with decreasing potential, the coiled PEG chains become loosened due to gradual desorption of the underlying Cl– adlayer.

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Section: Resultsmentioning

confidence: 98%

Section: Mound Model For Peg-clmentioning

confidence: 94%

Revisiting the Polyethylene Glycol-Chloride Adsorption Structure on Cu Electrode in Sulfuric Acid Solution by Wide-Frequency ATR-SEIRAS

Wu,

Mao,

Jiang

et al. 2023

J. Phys. Chem. C

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“…4. HS-AFM images of PEG adsorption on Au(100) at (a) -0.4 V, (b) -0.45 V, (c) -0.65 V, and (d) -0.75 V 11).…”

mentioning

confidence: 99%

<i>In-situ</i> Observation of Electrode Surface Change by High-Speed AFM

OHASHI,

MATSUSHIMA

2023

Vac. Surf. Sci.

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Dynamic behavior of electrochemical interfacial phenomena is key issue for material science. Scanning probe microscope can observe the surface on the nanoscale, however, it is difficult to discuss the reaction process due to poor temporal resolution. High-speed atomic force microscopy (HS-AFM) is one of powerful in-situ observation tools. Here, we would like to introduce the HS-AFM applications for electrochemistry, such as Cu electrodeposition, polyethylene glycol (PEG) adsorption, and nanobubble electrolytic evolution by HS-AFM.

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High‐Speed AFM Observation of Electrolytic Hydrogen Nanobubbles During Potential Scanning

Ohashi,

Ueda,

Matsushima

2024

Electrochemical Science Adv

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Nano‐sized bubbles (NBs: nanobubbles) have attracted attention in various fields such as physics, engineering, medicine and agriculture for fundamental and practical reasons. Atomic force microscopy (AFM) has revealed the occurrence of NBs and discovered their flattened shape. However, their dynamic behaviours have not yet been discussed much owing to the slow scanning speed. The existence of these energetically unfavourable structures is still controversial owing to the lack of studies on bubble‐like behaviour of NB such as aggregation, growth and dissolution. Recently developed high‐speed AFM (HS‐AFM) can observe nano‐interface phenomena at a speed of 0.5 frame s−1. In this study, HS‐AFM was applied to electrolytic H2 NBs. We successfully observed NB nucleation, growth and dissolution during a potential scan. Image analysis revealed flattened nuclei with heights of less than 10 nm. The NBs remained stable for a short period after the hydrogen evolution stopped, and they rapidly dissolved at the anodic potential. As the potential sweep was repeated, the number of NB nuclei increased. This is the first study showing the dynamic motion of NBs during the potential sweep by AFM. Videos captured by HS‐AFM make NB existence more certain. This research contributes not only to the NB study but also to the clarification of the gas evolution mechanism on electrodes.

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High Speed Atomic Force Microscope Observation of Polyethylene Glycol Adsorption on Au(100)

Cited by 3 publications

References 24 publications

Revisiting the Polyethylene Glycol-Chloride Adsorption Structure on Cu Electrode in Sulfuric Acid Solution by Wide-Frequency ATR-SEIRAS

Revisiting the Polyethylene Glycol-Chloride Adsorption Structure on Cu Electrode in Sulfuric Acid Solution by Wide-Frequency ATR-SEIRAS

<i>In-situ</i> Observation of Electrode Surface Change by High-Speed AFM

High‐Speed AFM Observation of Electrolytic Hydrogen Nanobubbles During Potential Scanning

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