Electrodeposition of Pd Intermetallics using Hg-In by the Electrochemical Liquid-Liquid-Solid Method

Wu, Haonan; Maldonado, Stephen

doi:10.1149/1945-7111/ac9bdc

Cited by 4 publications

(9 citation statements)

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“…This was placed at about L 2 = 40 cm from the sample in a position close to one of the tank walls. The webcam was controlled through the specialized SkyStudio Pro software [ 28 ] to take pictures every 10 minutes over the course of each experiment. The laser, lamp and electric motor (see Fig 1 ) were connected to an Arduino UNO board to control the switching on and off of each of these elements (more details on the electrical connections can be found in S2 Appendix ).…”

Section: Methodsmentioning

confidence: 99%

Accelerated corrosion of low carbon steel by oscillatory acidic streams generated with a bio-inspired claw device

Godínez,

Montoya-Rangel,

Montoya

2024

PLoS ONE

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A mechanical device inspired by the pistol shrimp snapper claw was developed. This technology features a claw characterized by a periodic opening/closing motion, at a controlled frequency, capable of producing oscillating flows at transitional Reynolds numbers. An innovative method was also proposed for determining the corrosion rate of carbon steel samples under oscillating acidic streams (aqueous solution of HCl). By employing very-thin carbon steel specimens (25 μm thickness), with one side coated with Zn and not exposed to the stream, it became possible to electrochemically sense the Zn surface once the steel sample was perforated, thus providing the average dissolution rate into the most relevant pit on the steel surface. Furthermore, a laser light positioned beneath the metallic sample, along with a camera programmed to periodically capture images of the steel surface, facilitated the accurate counting of the number of newly formed pits. The system consisting of the thin steel sample and the Zn coating can be seen as a type of corrosion sensor. Furthermore, the proposed laser illumination method allows corroborating the electrochemical detection of pits and also establishing their location. The techniques crafted in this study pave the way for developing alternative corrosion sensors that boast appealing attributes: affordability, compactness, and acceptable accuracy to detect in time and space localized damage.

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Section: Methodsmentioning

confidence: 99%

Accelerated corrosion of low carbon steel by oscillatory acidic streams generated with a bio-inspired claw device

Godínez,

Montoya-Rangel,

Montoya

2024

PLoS ONE

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“…For this purpose, we targeted the ec-LLS synthesis of In–Pd intermetallics . Such compounds are interesting as selective hydrogenation catalysts .…”

Section: Influence Of the Local Atomic Structure And Composition Of L...mentioning

confidence: 99%

Section: Influence Of the Local Atomic Structure And Composition Of L...mentioning

confidence: 99%

“…For this purpose, we targeted the ec-LLS synthesis of In−Pd intermetallics. 50 Such compounds are interesting as selective hydrogenation catalysts. 51 Simply melting solid In and solid Pd together will produce a variety of different compositions and phases, depending on the temperature and relative propor- These facts indicated an ec-LLS process featuring metal exchange between the nascent nuclei/crystals and the liquid metal solvent (Figure 7e).…”

Section: ■ Influence Of the Local Atomic Structure And Composition Of...mentioning

confidence: 99%

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Understanding and Expanding the Prospects for Electrosynthesis with Liquid Metal Electrodes

Hazelnis

Maldonado

2023

Acc. Chem. Res.

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Metrics & MoreArticle Recommendations CONSPECTUS: This Account describes and summarizes the latest work from our laboratory on developing and maturing strategies based on low-temperature liquid metals as reaction environments for materials synthesis. The electrochemical liquid−liquid−solid (ec-LLS) crystal growth concept is a hybrid method that combines electrodeposition and melt crystal growth. Using liquid metals as both electrodes and solvents for the purpose of producing inorganic crystals and materials, a simple and environmentally friendly process is possible. The impetus is to address the key deficiency in the inorganic crystalline materials that are the basis of modern optoelectronics and renewable energy capture/conversion systems. Specifically, existing methods for synthesizing crystalline inorganic materials for these purposes are largely energy-and resource-intensive, with a substantial impact on the environment when scaled. A long-term goal of our work with ec-LLS is to realize a materials synthetic process that is matured without requiring intensive resources or negatively impacting the environment. To this end, the factors that both limit and govern ec-LLS processes must be identified and understood. To date, questions regarding the factors that affect crystal nucleation and growth, form factors, and overall composition remain.Previous work established concretely ec-LLS as a versatile method for synthesizing and producing crystalline semiconductors at low temperatures as either particles, nanowires, or microwires. Subsequent experiments have focused on two tiers. First, the microscopic details of the liquid metal and its interfaces that dictate materials synthesis and crystal growth must be identified. Second, strategies that widen the attainable material form factors to facilitate device architectures must be realized. Hence, this Account describes results aimed at answering three questions: (1) What are the consequences of reaching supersaturation by an electrochemical rather than a thermal driving force for crystal growth in ec-LLS? (2) Can the location of nucleation and subsequent crystal growth be controlled? (3) Does the atomic structure of the liquid metal affect product formation in ec-LLS? The science described herein illustrates the value of in situ methods spanning transmission electron microscopy, X-ray diffraction, and X-ray reflectance for revealing the role that liquid metal composition and structure can play in ec-LLS. Additionally, we summarize work that shows for the first time that it is possible to produce both single-crystalline epitaxial films and complex intermetallic compounds through ec-LLS by tuning the cell design, electrochemical excitation waveform, and composition of the liquid metal electrodes.The cumulative findings described here substantially enrich our understanding of the ec-LLS concept while simultaneously motivating further questions moving forward. Is it possible to attain complete control over the crystalline quality and composition of ec-LLS products? Can th...

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“…Recently, an entirely different electrodeposition strategy for intermetallic synthesis was demonstrated that involved liquid metal electrodes [23] . Based off of the electrochemical liquid‐liquid‐solid (ec‐LLS) concept, [24] this recent report blended electroreduction with melt crystal growth.…”

Section: Introductionmentioning

confidence: 99%

Electrochemical Liquid‐Liquid‐Solid Growth of Ag‐In Crystals with Liquid Indium Alloy Electrodes

Wu,

Hazelnis,

Maldonado

2024

ChemElectroChem

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Synthesis of intermetallic crystals by electrodeposition of Ag from alkaline aqueous electrolytes containing AgCN onto liquid metal electrodes via an electrochemical liquid‐liquid‐solid (ec‐LLS) process has been performed. X‐ray diffraction, scanning electron microscopy, and transmission electron microscopy were performed to identify crystalline products. Ec‐LLS experiments performed with pure liquid Hg and Ga electrodes resulted in the formation of polycrystalline Ag2Ga and Ag2Hg3. Experiments performed with In‐containing liquid metals preferentially yielded Ag9In4 and AgIn2 products with liquid Hg0.35In0.65 and Ga0.86In0.14, respectively. The product distribution with liquid Hg0.35In0.65 depended on the level of Ag supersaturation during the electrodeposition. A mechanism that accounts for the aforementioned observations is presented and discussed. This work described the formation of Ag−In intermetallic phases by the isothermal electroreduction of Ag into different liquid metal solvents via ec‐LLS. Electrodeposition of Ag into a pure Ga or pure Hg liquid metal pool yielded precisely the compounds predicted from isothermal cross‐sections of the respective binary phase diagrams. These compounds were not found when using liquid Hg or Ga containing appreciable In. The smaller enthalpy of formation for AgIn2 was consistent with its synthesis in Ga0.86In0.14. However, the observed product of Ag9In4 in Hg‐containing liquid metals could not be rationalized solely from thermodynamic factors. Instead, this observation was consistent with a kinetic pathway based on the lability of Hg‐metal bonds and nearly identical crystal structures of Ag9In4 and Ag2Hg3. Site exchange of Hg for In is consistent with our prior observations[23] of In exchange into Hg−Pd structures during Pd electrodeposition. This mechanism is not based on any direct role of electrochemistry other than aspects that dictate the operative supersaturation of the metal solute.

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Electrodeposition of Pd Intermetallics using Hg-In by the Electrochemical Liquid-Liquid-Solid Method

Cited by 4 publications

References 61 publications

Accelerated corrosion of low carbon steel by oscillatory acidic streams generated with a bio-inspired claw device

Accelerated corrosion of low carbon steel by oscillatory acidic streams generated with a bio-inspired claw device

Understanding and Expanding the Prospects for Electrosynthesis with Liquid Metal Electrodes

Electrochemical Liquid‐Liquid‐Solid Growth of Ag‐In Crystals with Liquid Indium Alloy Electrodes

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