bluuebunny/crossref_metadata_2025_split huggingface dataset:
Electrodeposition of Microfabricated Rhenium-Filaments
Authors: Soule Luke , Coleman Jonathan , Pomerene Andrew , Arrington Christian L. , Petersen Steven 
Published: September 2023

Metallic filaments comprised of refractory materials are a necessary part of mass spectrometers used to measure isotopes. The current state-of-the-art material, rhenium, is formed into filaments using a mechanical crimper, limiting the accuracy, speed, and quantity of filaments that can be fabricated. The current work describes the development of wafer-scale, microfabricated Re filaments using silicon molds followed by electrodeposition of Re. The goal is to develop filaments with tight dimensional tolerances, high purity, and mechanical rigidity for the desired application and offer the ability to create 100’s-1000’s of filaments on a single silicon wafer.
Electrodeposition of Re is notoriously difficult as the reduction potential of rhenium is close to the hydrogen evolution reaction in aqueous solutions.1 While rhenium has been successfully deposited from alkaline, acid, and concentrated lithium chemistries,2 the films are often thin, porous, and contain many impurities such as hydrogen and oxygen. Rhenium oxide is susceptible to reaction with moisture in the air, resulting in poor quality films with short functional lifetimes. To electroform precise, pure rhenium structures, hardier chemistries must be developed.
The current work seeks to address this challenge using a water-in-salt chemistry (WISE) comprised of up to 4M lithium salts, complexing agents, reducing agents, and oxygen scavengers. Numerous physical agitation techniques were utilized to improve the quality of the film. Solutions were analyzed using various electrochemical techniques, UV-VIS, and Raman spectroscopy. The optimized chemistry was used to electrodeposit bulk batches of microfabricated 2mm x 300 um x 300 um filaments. The filaments were analyzed using microscopy, XRF, XRD, SEM, and EDS with a goal of use in high temperature mass spectrometry experiments.

References

(1) Naor, A.; Eliaz, N.; Burstein, L.; Gileadi, E. Direct Experimental Support for the Catalytic Effect of Iron-Group Metals on Electrodeposition of Rhenium. Electrochemical and Solid-State Letters
2010, 13 (12), D91. DOI: 10.1149/1.3489532.
(2) Pappas, D. P.; David, D. E.; Lake, R. E.; Bal, M.; Goldfarb, R. B.; Hite, D. A.; Kim, E.; Ku, H.-S.; Long, J.; McRae, C. Enhanced superconducting transition temperature in electroplated rhenium. Applied Physics Letters
2018, 112 (18), 182601.

Sandia National Laboratories is a multimission laboratory managed and operated by National Technology & Engineering Solutions of Sandia, LLC, a wholly owned subsidiary of Honeywell International Inc., for the U.S. Department of Energy’s National Nuclear Security Administration under contract DE-NA0003525. SAND2022-*****
Electrodeposition of Thin Films for Jewels and Fashion Accessories
Authors: Innocenti Massimo , Giurlani Walter , De Luca Antonio , Bonechi Marco , Comparini Andrea , Vorobyova Mariya Vorobyova , Verrucchi Margherita , Fontanesi Claudio , Caneschi Andrea 
Published: September 2023

The interest in scientific research within the metal finishing sector is growing. The demand for durable metals and adaptable manufacturing processes is increasing across a wide range of applications, from aerospace and automotive to machinery and jewelry. An essential step in the production line is the surface engineering of metals, as this determines the final appearance and functionality of a product. Therein electroplating is recognized as a mature technology allowing the low-cost fabrication of defined surfaces with extensive property profiles. Galvanic electrodeposition accounts today for almost 40% of the global market value share with North America and Western Europe leading the scenery. Although technological and processing advancements occurred in the past forty years, industrial firms are still struggling to provide solutions to corrosion protection as well as the reduction of toxic wastes. Specifically, large-scale industrialization of electroplating techniques will continue to be limited by strict environmental regulations. Due to adverse ecological impacts, the adoption of plating processes involving toxic metals such as lead or cadmium is prohibited. Moreover, price volatility of the highly demanding electroplated materials gold, copper, and nickel is expected to impact the market share by more than 60% by 2026.
In that respect, alloy plating offers better answers in terms of economic growth and environmental sustainability due to fine-tuning composition, morphology, and crystallinity [1]. Here, current trends in alloy electrodeposition research are reviewed highlighting open challenges and process innovations from an industrial perspective. The main categories of alloy compounds are presented and the most important properties of the manufacturing process are discussed. Particular attention is devoted to advances in industrial quality control and viable solutions for the reduction of precious metal content in electroplated accessories as well as the replacement of cyanide and nickel baths with non-toxic compounds.
The authors acknowledge Regione Toscana POR CreO FESR 2014-2020 – azione 1.1.5 sub-azione A1 – Bando 1 “Progetti Strategici di ricerca e sviluppo” which made possible the project:
“RAM-PVD” (CUP 3647.04032020.157000057_1225).

References

[1] W. Giurlani, M. Innocenti et all. , Electroplating for Decorative Applications: Recent Trends in Research and Development, Review, Coatings 2018, 8(8), 260.
Additive Manufacturing of Inductors and Transformers by Hybrid Aerosol Jet Printing and Electrochemical Deposition
Authors: Tsui Lok-kun , Sui Yongkun , Hartmann Thomas Michael , Dye Joshua , Lavin Judith Maria 
Published: September 2023

Aerosol jet printing (AJP) is an attractive additive manufacturing process for printed electronic applications due to its high resolution (< 10 µm), flexible stand-off distance, and support of both metal and dielectric materials. A slow deposition rate (< 1 µm per layer) and the relatively low conductivity achievable with commercially available nanoparticle inks (~40% bulk) present some of the current limitations associated with AJP. Electrochemical deposition methods including both electrodeposition and electroless deposition are widely used in the microelectronics industry. Dense, high conductivity layers several 10s of µm can be deposited with well-established plating processes. Metals including Cu and Ni which are challenging to deposit by AJP, can be easily/readily deposited using commercially available plating baths. A hybrid approach of seed layer deposition using AJP and electrochemical deposition of highly conductive copper is used to improve the overall conductance of the printed structures. [1] Here, we apply this combined approach to the manufacturing of transformer and inductor devices.
We have successfully prepared a two-layer secondary inductor on top of a two-layer primary inductor to form a coreless flyback transformer (Figure 1(a)). These inductors were fabricated by AJP of an Ag seed layer, followed by electroless deposition and electrodeposition of Cu and Ni. UV-curable dielectric polymer layers were deposited by AJP to separate each inductor layer. The flyback transformer produced a gain of 75.3x with an input voltage of 17 V at 400 kHz resulting in an output voltage of 1250 V (Figure 1(b)). We also demonstrated the repeated stacking of 8 coil layers by AJP of Ag seed layers and electrodeposition of Cu and Ni (Figure 1(c)). These inductors had an average equivalent series resistance of 0.6 Ω and a 1.7 µH inductance at 100 kHz (Figure 1(d)). Finally, we will study the deposition of these inductor and transformer devices on magnetic substrates, characterizing changes in inductance and gain.

SNL is managed and operated by NTESS under DOE NNSA contract DE-NA0003525. SAND2022-17001 A

References:

[1] L. Tsui, S.C. Kayser, S.A. Strong, J.M. Lavin. ECS J. Solid State Sci. Technol. 10 (2021) 047001.

Figure 1. (a) Additively manufactured coreless flyback transformer fabricated by combined aerosol jet printing, electroless deposition, and electrodeposition. (b) Output voltage vs. input voltage at 400 kHz resulting in a gain of 73.5x. (c) 8-layer inductor fabricated by combined aerosol jet printing and electrodeposition. (d) Inductance at 100 kHz as a function of number of layers for the multi-layer inductor up to 8 layers.

Figure 1
Tunable Conformal Electrodeposition of Ultra-Thin Polymeric Films for Electrolyte Interphases
Authors: Wang Wenlu , Resing Anton B , Zheng Zhaoyi , Brown Keith A , Werner Joerg G 
Published: September 2023

Functional coatings and interphases influence the stability and performance parameters of electrodes in various applications. Polymer thin films offer a wide range of molecular structures and compositions for tunable functionalities that can be custom designed to the needs of an application. In solid-state energy storage devices in particular, electrolyte-type polymeric interfaces between battery components and materials with disparate functions, such as the active electrode material and solid electrolyte could overcome some of these incompatibility detriments and the increase in contact resistance over long-term operation. In high-performance micro scale power sources, 3D thin-film all-solid-state batteries show great potential as they take advantage of both short ion diffusion distances for high-rate capability with low heat generation, as well as the third dimension for high material loading and energy density. Therefore, conformal deposition methods for ultra-thin polymeric electrolyte interphases on the interior surface of electrodes with mesoscale 3D architectures and complex porosity are in demand.
Here, we report a molecular design concept of dual-functional molecules that contain electrochemically active end groups for self-limiting electropolymerization, and a core molecular motif that determines the thin film functionality. The electrodeposition of this monomer represents a non-line-of-sight coating method for polymer thin films with independently tailorable functionalities and tunable properties on conductive substrates with arbitrary shape.
We exemplify this method using monomers with poly(ethylene glycol) (PEG) as the core motif for lithium-ion transport and phenol as electrochemically active end groups. We studied the electrodeposition of the monomers, poly(ethylene glycol) diphenol (PEGDP), and demonstrate their self-limiting film formation mechanism (Figure 1a) which originates from the insulating nature of resulting poly(PEGDP) film that confines the charge transfer reaction. We present an exhaustive exploration of their material-processing-structure-property relationships that reveals the multi-scale control over the ultrathin-film properties. For example, the uniform film thickness is tunable from 10 to 100s of nanometer through electrodeposition conditions and molecular design, while their molecular permeability and electronic resistance can be tailored from pervious to fully blocking. We show that the electrodeposited functional interphases fully coat complex 3D electrode architectures (Figure 1b top: uncoated carbon electrode, bottom: film coated carbon electrode) with retention of their functionality in a battery. This work demonstrates that rational molecular design enables the conformal electrodeposition of ultrathin functional coatings with solid polymer electrolyte properties on 3D structured electrodes that will enable designer interphases in various solid-state battery architectures and chemistries.

Figure 1
An Electrochemical and Spectroscopic Characterization of Chiral MIL-53(Fe) Metal-Organic Framework
Authors: Bonechi Marco , Bettoni Diana , Maccioni Irene , Biffoli Fabio , Giurlani Walter , Salzillo Tommaso , Kawondera Rufaro , Mtangi Wilbert , Fontanesi Claudio , Innocenti Massimo 
Published: September 2023

Metal-organic frameworks (MOFs) have attracted increasing scientific interest due to unique features including high specific surface areas, exceptional porosity, high crystallinity and tuneable pore size [1]. In fact, the opportunity to achieve porous materials with high modularity and diverse functionality make MOFs suitable candidate for solid-state materials. In recent years, scientists conducted intense research in the production of chiral MOFs (CMOFs). The attractiveness of chiral MOFs is due to their specific application including chiral enantioselective recognition, enantioselective separation, asymmetric catalysis, and sensing. Chirality within MOFs can occur in each of the components, whether linker, metal node, or even guest molecules [2]. MIL-53(Fe) is the most common iron-based MOF. This class of compound is obtained by a combination between iron(III) cations and 1,4-dicarboxylic acid consists of three-dimensional networks which contain FeO6 hexagonal chains and dicarboxylate anions. MIL-53(Fe) shows significant advantages compared with other MOFs, which include chemical stability, the presence of nontoxic and widely available metals [3]. MIL-53(Fe) derivatives containing chiral molecules (cysteine and camphorsulfonic acid) were characterized by IR, XRD and Electron Spectroscopy. The electrochemical behaviour of the synthesized MOFs was characterized on solid state using a glassy carbon (GC) electrode and by making a paste with graphite powder. Cyclic voltammetry (CV) measurements show different redox behaviour depending on the type of molecules present inside the framework. The experimental results were integrated and related to the properties obtained using DFT based quantum mechanical calculations.

References

[1] Q. Wang, D. Astruc, Chem. Rev.
2020, 120, 1438–1511
[2] Z. Sharifzadeh, K. Berijani, A. Morsali, Coordination Chemistry Reviews
2021, 445, 214083
[3] F. Millange, R. I. Walton, Israel Journal of Chemistry
2018, 58, 1019–1035
Porous Copper Layer Development by Dynamic Hydrogen Bubble Template for Power Modules Assembling by Thermocompression
Authors: Schoenleber Jonathan , Chachay Lucas , Janod Goulven , Gigandet Marie-Pierre , Hihn Jean-Yves , Daudin Remi , Missiaen Jean-Michel , Bouvard Didier , Avenas Yvan , Khazaka Rabih 
Published: September 2023

Copper is the most widely used materials for microelectronics applications due to their electrical and thermal conduction properties, and in several applications, thick and porous layers are requested. With increased aircraft electrification, there is a need of extremely high-power converters in the power electric chain, interfacing the bus and the electric motor. The COPERPACK project (COPPER based PACKaging for direct cooled power module ANR-19-CE05-0011) aims to module assembling by thermocompression, which requested the elaboration of thin nanoporous copper film to be placed between chips and metallized ceramic substrates.
Different possibilities still exists such as copper-zinc or copper-manganese electrodeposition followed by an anodic dissolution, but the faster and simpler way resides in electroforming deposition made by Dynamic Hydrogen Bubble Template (DHBT) [1]. This process works in unusual potentials and current densities where the competition between hydrogen discharge (commonly avoided) and copper reduction is very high. In this case, this method achieves thick deposits in very short time (few seconds) with high currents allowing a very fast growth of copper around hydrogen bubbles. Pores and ligaments sizes can be controlled by several operating parameters i.e. current densities, temperature, deposit time, chemical additives [2] as well by pulsed currents. Films were tested for chips assembling by thermocompression, and present excellent behavior’s.
[1] Abdel-Karim, R.; El-Raghy, S. Chap 4 in Advanced materials and their applications - micro to nano scale. One Central Press, United Kingdom, pp 69–91, 2017
[2] Shin, H.-C.; Liu, M. Chem. Mater. 2004, 16, 25, 5460–5464 doi.org/10.1021/cm048887b

Figure 1
In-Situ Li Plating Reactions on Inorganic Solid Electrolytes for Advanced All-Solid-State Batteries
Authors: Iriyama Yasutoshi 
Published: September 2023

All-solid-state batteries (SSBs) using lithium metal anode are expected to realize SSBs with high energy density. This is because lithium metal anode has the lowest redox potential and the theoretical capacity of 3861 mA h g-1 is ca. ten times larger than that of commonly-used graphite anode (372 mA h g-1). In fact, lithium metal anode has been successfully used in thin-film-type SSBs and stable charge-discharge reactions are reported [1]. In SSBs, both positive and negative electrode materials are combined with solid electrolytes, and they are assembled from the initial state in general. On the other hand, conventional SSBs apply lithium transition metal oxides (LiCoO2, etc.) as the positive electrode material, and lithium metal is electrochemically plated during the charging process. Appling electrochemically-plated lithium as a anode material can simplify the battery manufacturing process and will be an effective way to form pure lithium metal anode. Such “Li-free” SSBs has been successfully prepared in thin-film-type SSBs [2]. Also, this anode-less idea has been applied to develop large-sized SSBs in recent years [3].
In this presentation, the author will talk about the factors for lithium plating morphology on inorganic solid electrolytes, such as current collector species, current densities, temperature, etc. [4]. The model solid electrolytes are LiPON-coated LATP or garnet-structured Ta-doped LLZ. Also, several problems for applying electrochemically-plated lithium anode and the issues arising during the stripping processes will be discussed.
References
[1] J. B. Bates, N. J. Dudney, B. Neudecker et al., Solid State Ionics
135 (2000) 33.
[2] B. J. Neudecker, N. J. Dudney, and J. B. Bates, J. Electrochem. Soc.
147 (2000) 517.
[3] a) Y-G. Lee, S. Fujiki, C. Jung, et al., Nature Energy
5 (2020) 299. b) https://www.quantumscape.com/ 2020/12/16
[4] a) F. Sagane, K-I. Ikeda, Y. Iriyama et al., J. Power Sources
233 (2013) 34. b) F. Sagane, R. Shimokawa, Y. Iriyama et al., J. Power Sources
225 (2013) 245. c) M. Motoyama, M. Ejiri, and Y. Iriyama, J. Electrochem. Soc.
162 (2015) A7067. d) F. Yonemoto, A. Nishimura, Y. Iriyama et al., J. Power Sources
343 (2017) 207. e) M. Motoyama, M. Ejiri, Y. Iriyama et al., J. Electrochem. Soc.
165 (2018) A1338. f) T. Yamamoto, H. Iwasaki, Y. Iriyama et al., Electrochem. Comm.
105 (2019) 106494.
Combining 1D and 3D Multi-Physics Modeling Methodologies for Thermal Runaway Propagation Analysis
Authors: Pisharodi Vivek , Artukovic Dominik , Holcomb Brad , Gundlapally Santhosh , Biju Nikhil , Luo Gang , Wimmer Joe 
Published: September 2023

Battery pack designers must ensure that all battery packs are designed to withstand a single cell entering thermal runaway without the heat from this cell causing thermal runaway to occur in neighboring cells, leading to thermal runaway propagation. Pack designers must be confident that no matter which cell enters thermal runaway, and no matter how the cell enters thermal runaway, that thermal runaway will not propagate into a pack-level fire.
Studying thermal runaway events at the pack-level has historically relied heavily on expensive pack-level experimental tests using prototype batteries or computationally-expensive 3D CAE analyses. Because the cost of a single test in either scenario (real cost or computational cost) is very high, both options allow for only a handful of scenarios to be realistically studied.
Additionally, when reduced-order models of pack-level thermal runaway are employed, they have historically relied on empirically-driven models for the heat generation of cells entering thermal runaway. These models often rely on knowing the heat ejected from a cell ahead of time and often ignores the history of cells leading up to their thermal runaway events.
This presentation will demonstrate the benefits of a physics-driven approach to reduced-order modelling of pack-level thermal runaway propagation. By combining 1D/3D thermal structure modelling of cell temperature, 1D flow simulation of flow paths between cells, pseudo-2D electrochemical modelling of cells leading up to thermal runaway, and generalized chemical modelling for thermal runaway reactions inside the cell, this presentation demonstrates a computationally efficient approach to modeling thermal runaway propagation that also has high model fidelity and accuracy.
With an accurate and fast-running model, more virtual experiments can be setup to enable more what-if scenarios to be tested. This includes robust case sweeps and even multi-factor design of experiments (DoE) tests to be done.
Gold Electropolishing Using Cyanide-Free Electrolytes
Authors: Rodriguez Julymar del Carmen , Doche Marie-Laure , Hihn Jean-Yves 
Published: September 2023

Electropolishing or electrochemical polishing (EP), is an ultrafinishing process that improves the aesthetic, technical and functional properties of surfaces by reducing their roughness. This process is based on the anodic dissolution of the workpiece through an oxidation reaction. The polishing effect is due to the formation of a viscous layer that induces a preferential dissolution of the peaks of the surface profile at the expense of the valley. This results in the surface leveling and in brightness improvement. Compared to conventional mechanical finishing techniques, EP is a non-contact process that does not disturb the metallurgy of the surface layer. In addition, it allows the treatment of relatively complex geometries as well as the obtention of reproducible results.
Regarding the electrolyte composition, it often includes oxidizing agents to activate the anodic dissolution (strong acids, hydrogen peroxide, ...) as well as depassivating agents to prevent the oxide film from becoming too stable (halides, alcohols, ...) and viscous layer promoting agents (glycerol, organic acids, ...). In the case of gold, the presence of a complexing agent lowers the oxidation potential and facilitates dissolution. However, most of the electrolytes used for EP of precious metals are toxic due to the presence of cyanides or thiourea. Furthermore, each alloy requires a specific electrolyte formulation and therefore suitable operating parameters. The complexity of the mechanisms involved and the associated environmental risks make it difficult to deploy this technique in the luxury and jewelry industry. Another concern is the lack of literature regarding the role of each component.
A better understanding of the process could lead to an improvement of the electrolyte formulation and to the proposal of other options with a lower environmental impact. The aim of this work is to study the effect of various non-toxic and ecofriendly electrolytes on the electropolishing mechanisms of gold and gold alloys. Their efficiency will be evaluated in terms of the surface properties obtained after the treatment: roughness reduction (macro/micro) and gloss. Moreover, the effect of each component of the electrolytes is investigated using electrochemical measurements, in the perspective of describing EP mechanism and its consequences on surface properties.

Figure 1