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At least 37 records · Page 2

One-Step Spark Plasma Erosion Processing of Carbon-Coated Sn-Si Nanoparticles for Lithium-Ion Battery Anodes

High density portable energy storage is desirable owing to the energy requirements of portable electronics and electric vehicles. The Li-ion battery’s high energy density could be even further improved through the utilization of alternative materials (instead of carbon) for the anode, such as Sn or Si. Nonetheless, the large volume expansion upon lithiation, up to ~300% for Li 22 Si 5 , causes pulverization and rapid capacity degradation during cycling. Sn also forms a Li 22 Sn 5 compound with the equivalent stoichiometric Li capacity but with enhanced ductility. Nano-sized Si and Sn have demonstrated distinctive nanoscale properties, facilitating the retention of higher capacities, particularly when coated with carbon, which improves mechanical stability. To date, the methods of synthesizing coated Si, Sn, or Si-Sn alloyed nanoparticles are complicated, costly, and not readily scalable to meet the demands of cost-effective manufacturing. Spark plasma erosion in a hydrocarbon dielectric has been explored as a one-step process to produce Sn-Si alloy nanoparticles coated with a thin carbon film, offering a scalable and cost-effective processing route. The resulting Sn-Si particles exhibited a bi-modal size distribution at ~5 nm and ~500 nm and were carbon-coated, as intended, from the hydrocarbon dielectric breakdown. The spark-eroded nanoparticles were thoroughly characterized using TEM/EDS, XPS, AES, SSNMR, and TGA, and their improved electrochemical performance was assessed through half-cell experiments.

25 ENERGY STORAGE↗

Optimization of Nb 3 Sn sputtering on SRF structures

Superconducting radiofrequency (SRF) cavities are the key technology to compact, high-efficiency, and cost-effective CW SRF accelerators. Further improvements in the efficiency can be realized by using novel materials such as Nb 3 Sn coated on the inner surface of SRF cavities. The Nb 3 Sn coatings enable cavity operation at 4 K, where the Nb 3 Sn coated cavities are already very efficient and have high intrinsic quality factors. Advances in Nb3Sn coatings on the inner surface of SRF cavities showed the potential for this material to significantly cut the capital and operating costs of SRF accelerators. Several approaches have been and are being investigated for coating SRF cavities with Nb 3 Sn. Magnetron sputtering is a versatile technique in that it has been shown to produce Nb 3 Sn films on flat Nb target in a single phase and a precisely controlled thickness, low defect levels, and a favorable morphology. Deposition of Nb 3 Sn films on SRF cavities have also shown promising RF superconducting properties. However, sputter coating of Nb 3 Sn on SRF cavities requires further development to be used in accelerators.

43 PARTICLE ACCELERATORS↗

Sputter coating of Nb₃Sn into SRF cavity using stoichiometric target

Nb₃Sn has emerged as a leading alternative material due to its higher superconducting critical temperature (Tc) and superheating field (Hsh), promising a viable solution to the intrinsic performance limit currently faced by Nb superconducting radiofrequency (SRF) cavities. We sputter-coated Nb₃Sn inside Nb SRF cavity using a stoichiometric Nb₃Sn tube target in a DC cylindrical magnetron sputter coater. The target was fabricated by growing an estimated >20 μm thick Nb₃Sn layer on a Nb tube via Sn vapor diffusion using Jefferson Lab’s coating system. Approximately 150 nm thick Nb-Sn films were sputter-deposited onto flat Nb samples at positions representing the beam tubes and equator of a 2.6 GHz Nb cavity. Post-deposition annealing at 950 °C for 3 h resulted in the formation of Nb₃Sn. Microstructural analysis of the annealed films was carried out to investigate the morphology and structure of the Nb₃Sn films. Later, a 2.6 GHz Nb SRF cavity was coated with a ~1.2 μm thick sputtered Nb-Sn film using a stoichiometric Nb₃Sn target, followed by annealing. Cryogenic RF testing of the annealed cavity demonstrated a Tc of 17.8 K, indicating the formation of Nb₃Sn. After a light Sn recoating treatment, the cavity achieved a quality factor (Q0) of 6.7E+08 at lower field at 2.0 K.

Accelerator Physics↗

In operando X-ray diffraction strain measurement in Ni 3 Sn 2 – Coated inverse opal nanoscaffold anodes for Li-ion batteries

Volume changes associated with the (de)lithiation of a nanostructured Ni 3 Sn 2 coated nickel inverse opal scaffold anode create mismatch stresses and strains between the Ni 3 Sn 2 anode material and its mechanically supporting Ni scaffold. By using in operando synchrotron x-ray diffraction measurements, elastic strains in the Ni scaffold are determined during cyclic (dis)charging of the Ni 3 Sn 2 anode. These strains are characterized using both the center position of the Ni diffraction peaks, to quantify the average strain, and the peak breadth, which describes the distribution of strain in the measured volume. Upon lithiation (half-cell discharging) or delithiation (half-cell charging), compressive strains and peak breadth linearly increase or decrease, respectively, with charge. The evolution of the average strains and peak breadths suggests that some irreversible plastic deformation and/or delamination occurs during cycling, which can result in capacity fade in the anode. The strain behavior associated with cycling of the Ni 3 Sn 2 anode is similar to that observed in recent studies on a Ni inverse-opal supported amorphous Si anode and demonstrates that the (de)lithiation-induced deformation and damage mechanisms are likely equivalent in both anodes, even though the magnitude of mismatch strain in the Ni 3 Sn 2 is lower due to the lower (de)lithiation-induced contraction/expansion.

25 ENERGY STORAGE↗

Managing Sn-Supply to Tune Surface Characteristics of Vapor-Diffusion Coating of Nb₃Sn

Nb₃Sn promises better RF performance (Q and E_{acc}) than niobium at any given temperature because of superior superconducting properties. Nb₃Sn-coated SRF cavities are now produced routinely by growing a few microns thick Nb₃Sn films inside Nb cavities via the tin vapor diffusion technique. Sn evaporation and consumption during the growth process notably affect the quality of the coating. Aiming at favorable surface characteristics that could enhance the RF performance, many coatings were produced by varying Sn sources and temperature profiles. Coupon samples were examined using different material characterization techniques, and a selected few sets of coating parameters were used to coat 1.3 GHz single-cell cavities for RF testing. The Sn supply’s careful tuning is essential to manage the microstructure, roughness, and overall surface characteristics of the coating. We summarize the material analysis of witness samples and discuss the performance of several Nb₃Sn-coated single-cell cavities linked to Sn-source characteristics and observed Sn consumption during the film growth process.

Pudasaini, U.↗

Can a Coating Mitigate Molten Na Dendrite Growth in NaSICON Under High Current Density?

Alkali metals are among the most desirable negative electrodes for long duration energy storage due to their extremely high capacities. Currently, only high-temperature (>250 °C) batteries have successfully used alkali electrodes in commercial applications, due to limitations imposed by solid electrolytes, such as low conductivity at moderate temperatures and susceptibility to dendrites. Toward enabling the next generation of grid-scale, long duration batteries, we aim to develop molten sodium (Na) systems that operate with commercially attractive performance metrics including high current density (>100 mA cm –2 ), low temperature (<200 °C), and long discharge times (>12 h). In this work, we focus on the performance of NaSICON solid electrolytes in sodium symmetric cells at 110 °C. Specifically, we use a tin (Sn) coating on NaSICON to reduce interfacial resistance by a factor of 10, enabling molten Na symmetric cell operation with “discharge” durations up to 23 h at 100 mA cm –2 and 110 °C. Unidirectional galvanostatic testing shows a 70% overpotential reduction, and electrochemical impedance spectroscopy (EIS) highlights the reduction in interfacial resistance due to the Sn coating. Detailed scanning electron microscopy (SEM) and energy-dispersive spectroscopy (EDS) show that Sn-coated NaSICON enables current densities of up to 500 mA cm –2 at 110 °C by suppressing dendrite formation at the plating interface (Mode I). In conclusion, this analysis also provides a mechanistic understanding of dendrite formation at current densities up to 1000 mA cm –2 , highlighting the importance of effective coatings that will enable advanced battery technologies for long-term energy storage.

25 ENERGY STORAGE↗

Superconducting low-beta Nb 3 Sn cavity for ATLAS and future ion accelerators

We report on a Nb 3 Sn-coated low-beta superconducting radio frequency (RF) cavity intended for accelerating ions. We aim to apply the cavity in ATLAS, our Argonne National Laboratory user facility for nuclear physics studies with ion beams in the energy range of 5–20 MeV u −1 . The Nb 3 Sn-coated cavity, a 145 MHz quarter-wave optimized for ions moving with velocity β = $v/c$ = 0.08 exhibits an order-of-magnitude reduction in RF losses into helium at 4.4 K compared to a superconducting niobium (Nb) cavity at the same frequency and temperature. Experimentally measured fields are among the highest to date for any Nb 3 Sn-coated cavity, reaching a peak surface magnetic field of 105 mT. We also present a practical solution to the problem of cavity frequency tuning. Tuning by mechanical deformation has been a challenge with Nb 3 Sn due to its brittle nature, however, using a set of techniques tailored to the properties of thin-film Nb 3 Sn on Nb, we can repeatably tune the cavity to the ATLAS master clock frequency after it is cooled, while maintaining the excellent performance characteristics. The same Nb 3 Sn cavity technology offers broad benefits for future ion accelerators.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Challenges of Vapor Diffusion $Nb_3Sn$ Coating at Fermilab: Minimizing Impurities Using TOF-SIMS

Nb$_3$Sn demonstrates steady advancements nowadays offering reduced power cost in superconducting radio-frequency cavities due to its high critical temperature, quality factor, and achieved accelerating gradient. However, theoretical estimates of its radio-frequency parameters have not been achieved due to several potentially limiting mechanisms: tin spots, patchy regions, defects, thermal impedance, and impurities. While some of these limitations have been intensively studied, impurity analysis in Nb$_3$Sn coatings have received less attention. We report an investigation of impurities in several vapor-diffused Nb$_3$Snn coated samples using time-of-flight secondary ion mass spectroscopy (TOF-SIMS) and show allowable impurity levels in view of superconducting cavity performance. Challenges and lessons learned in maintaining clean Nb$_3$Sn coatings are also discussed.

Tagdulang, N. [Fermilab]↗

Mitigation of tin whisker growth by inserting Ni nanocones

Highlights: • Tin whisker growth is mitigated effectively by inserting Ni nanocones. • Ni nanocones impede Sn dynamic recrystallization by blocking dislocation motions. • The inhibition method and mechanism are important to the study of tin whisker. - Abstract: An innovative controllable way has been proposed to mitigate tin whisker growth by inserting Ni nanocones prepared by electrodeposition. The results reveal that, after inserting Ni nanocones, tin whisker formation is mitigated effectively for 1.6 μm Sn coating but there is no inhibition effect for 4.5 μm Sn coating. The coatings are characterized by X-ray diffraction, scanning electron microscopy, energy dispersive spectrometer and electron backscatter diffraction (EBSD). The EBSD results show that Sn grain size without Ni nanocones increases significantly after indentation test compared with Sn grains with Ni nanocones. The inhibition effect of Ni nanocones on whisker growth can be ascribed to its specific structure which prevents dynamic recrystallization and produces horizontal grain boundaries of Sn grains. The structural inhibition method and mechanism proposed are of great importance to the research of tin whisker.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Co-Sputtering of Nb3Sn into SRF Cavity Using Composite Target and Optimizing Surface Homogeneity

Nb₃Sn coating method for superconducting radiofrequency (SRF) cavity has been developed following co-sputtering of Nb-Sn composite target using a DC cylindrical sputter coater. Deposition parameters and annealing strategies were optimized for uniform Nb₃Sn coating. 1.5 m Nb-Sn film was deposited onto 2.6 GHz Nb SRF cavity and annealed at 600 C for 6 h, followed by 950 C for 1 h. Cryogenic RF testing confirmed Nb₃Sn formation with Tc = 17.8 K. A post-annealing light Sn recoating process improved the cavity s performance, achieving Q₀ = 8.5 10⁸ at 2.0 K.

Shakel, M. S. [Old Dominion U.]↗

Dynamic Recrystallization Model for Whisker and Hillock Growth

Tin (Sn) whiskers are not a recent development. Studies in the late 1930’s investigated thin filaments that grew spontaneously from Sn coatings used for the corrosion protection of electronic hardware. It was soon recognized that these Sn filaments, or whiskers, could create short circuits in the same electronic equipment. Figure 1a illustrates whisker growth in the hole of a printed circuit board having an immersion Sn surface finish. The engineering solution was to contaminate the Sn with > 3 wt.% of lead (Pb). The result was that whisker growth was replaced with hillock formation (Fig. 1b) that posed a minimal reliability concern to electrical circuits. Today, Pb-containing finishes are being replaced with pure Sn coatings to meet environmental restrictions on Pb use. The same short-circuit concerns have been raised, once again, with respect to Sn whiskers.

Vianco, Paul T.↗

Dynamic Recrystallization Model for Whisker and Hillock Growth

Tin (Sn) whiskers are not a recent development. Studies in the late 1930’s investigated thin filaments that grew spontaneously from Sn coatings used for the corrosion protection of electronic hardware. It was soon recognized that these Sn filaments,or whiskers, could create short circuits in the same electronic equipment. Figure 1a illustrates whisker growth in the hole of a printed circuit board having an immersion Sn surface finish. The engineering solution was to contaminate the Sn with > 3wt.% of lead (Pb). The result was that whisker growth was replaced with hillock formation (Fig. 1b) that posed a minimal reliability concernto electrical circuits. Today, Pb-containing finishes are being replaced with pure Sn coatings to meet environmental restrictions on Pb use. The same short-circuit concerns have been raised, once again, with respect to Sn whiskers. The present authors have taken the approach that, in order to develop more widely applicable, first-principles strategies to mitigate Sn whisker formation, it is necessary to understand the fundamental mechanism(s) and rate kinetics underlying their development. Numerous mechanisms have been proposed by other authors to describe whisker growth, including static recrystallization by Boguslavsky and Bush.

36 MATERIALS SCIENCE↗

Atomic-scale analyses of Nb 3 Sn on Nb prepared by vapor diffusion for superconducting radiofrequency cavity applications: a correlative study

We report on atomic-scale analyses of the microstructure of an Nb 3 Sn coating on Nb, prepared by a vapor diffusion process for superconducting radiofrequency (SRF) cavity applications using transmission electron microscopy, electron backscatter diffraction and first-principles calculations. Epitaxial growth of Nb 3 Sn on a Nb substrate is found and four types of orientation relationships (ORs) at the Nb 3 Sn/Nb interface are identified by electron diffraction or high-resolution scanning transmission electron microscopy (HR-STEM) analyses. Thin Nb 3 Sn grains are observed in regions with a low Sn flux and they have a specific OR: Nb 3 Sn (1$\bar{2}$0) //Nb ($\bar{1}$11) and Nb 3 Sn (002) //Nb (0$\bar{1}$1) The Nb 3 Sn/Nb interface of thin grains has a large lattice mismatch, 12.3%, between Nb(0$\bar{1}$1) and Nb 3 Sn (002) and a high density of misfit dislocations as observed by HR-STEM. Based on our microstructural analyses of the thin grains, we conclude that the thin regions are probably a result of a slow interfacial migration with this particular OR. The Sn-deficient regions are seen to form initially at the Nb 3 Sn/Nb interface and remain in the grains due to the slow diffusion of Sn in bulk Nb 3 Sn. The formation of Sn-deficient regions and the effects of interfacial energies on the formation of Sn-deficient regions at different interfaces are estimated by first-principles calculations. The finding of ORs at the Nb 3 Sn/Nb interface provides important information about the formation of imperfections in Nb 3 Sn coatings, such as large thin-regions and Sn-deficient regions, which are critical to the performance of Nb 3 Sn SRF cavities for accelerators.

43 PARTICLE ACCELERATORS↗

First Results from A $Nb_3Sn$-Coated 1.5-Cell 650MHZ SRF Cavity for Cryogen-Free Industrial Accelerators

Fermilab is advancing the development of a compact, high-power electron beam accelerator using superconducting radio frequency (SRF) technology as a non-radioactive alternative to traditional radiological sources. The current design targets continuous-wave (CW) operation at \SI{1.6}{MeV} and \SI{20}{kW}. To ensure suitability for industrial environments, the system is being designed for cryogen-free operation, driving the adoption of a novel Nb$_3$Sn-coated 1.5-cell SRF cavity operating at \SI{650}{MHz}. This contribution reports on the fabrication, surface preparation, and Nb$_3$Sn coating process of the cavity, as well as first results from vertical test stand (VTS) measurements performed in a liquid helium bath. These initial tests mark a key milestone toward demonstrating the viability of conduction-cooled Nb$_3$Sn SRF cavities for industrial-scale deployment.

Tagdulang, Nikki Diala [Fermilab]↗

First Results from a Nb3Sn-Coated 1.5-Cell 650 MHz SRF Cavity for Cryogen-Free Industrial Accelerators

First Results from a Nb3Sn-Coated 1.5-Cell 650 MHz SRF Cavity for Cryogen-Free Industrial Accelerators ABSTRACT = Fermilab is advancing the development of a compact, high-power electron beam accelerator using superconducting radio frequency (SRF) technology as a non-radioactive alternative to traditional radiological sources. The current design targets continuous-wave (CW) operation at \SI{1.6}{MeV} and \SI{20}{kW}. To ensure suitability for industrial environments, the system is being designed for cryogen-free operation, driving the adoption of a novel Nb$_3$Sn-coated 1.5-cell SRF cavity operating at \SI{650}{MHz}. This contribution reports on the fabrication, surface preparation, and Nb$_3$Sn coating process of the cavity, as well as first results from vertical test stand (VTS) measurements performed in a liquid helium bath. These initial tests mark a key milestone toward demonstrating the viability of conduction-cooled Nb$_3$Sn SRF cavities for industrial-scale deployment.

Tagdulang, N. [Fermilab]↗

Degradation-resistant TiO 2 @Sn anodes for high-capacity lithium-ion batteries

As the demand for higher-performance batteries has increased, so has the body of research on theoretical high-capacity anode materials. However, the research has been hindered because the high-capacity anode material properties and interactions are not well understood, largely due to the difficulty of observing cycling in situ. Using electrochemical scanning transmission electron microscopy (ec-STEM), we report the real-time observation and electrochemical analysis of pristine tin (Sn) and titanium dioxide-coated Sn (TiO 2 @Sn) electrodes during lithiation/delithiation. As expected, we observed a volume expansion of the pristine Sn electrodes during lithiation, but we further observed that the expansion was followed by Sn detachment from the current collector. Remarkably, although the TiO 2 @Sn electrodes also exhibited similar volume expansion during lithiation, they showed no evidence of Sn detachment. We found that the TiO 2 surface layer acted as an electrochemically activated artificial solid-electrolyte interphase that serves to conduct Li ions. As a physical coating, it mechanically prevented Sn detachment following volume changes during cycling, providing significant degradation resistance and 80% Coulombic efficiency for a complete lithiation/delithiation cycle. Interestingly, upon delithiation, TiO 2 @Sn electrode displayed a self-healing mechanism of small pore formation in the Sn particle followed by agglomeration into several larger pores as delithiation continued.

25 ENERGY STORAGE↗

Modeling of Stresses and Strains during (De)Lithiation of Ni 3 Sn 2 -Coated Nickel Inverse-Opal Anodes

Tin alloy-based anodes supported by inverse-opal nanoscaffolds undergo large volume changes from (de)lithiation during cyclic battery (dis)charging, affecting their mechanical stability. In this work we perform continuum mechanics-based simulation to study the evolution of internal stresses and strains as a function of the geometry of the active layer(s): (i) thickness of Ni 3 Sn 2 single layer (30 and 60 nm) and (ii) stacking sequence of Ni 3 Sn 2 and amorphous Si in bilayers (60 nm thick). For single Ni3Sn2 active layers, a thinner layer displays higher strains and stresses, which are relevant to mechanical stability, but causes lower strains and stresses in the Ni scaffold. For Ni 3 Sn 2 -Si bilayers, the stacking sequence significantly affects the deformation of the active layers and thus its mechanical stability due to different lithiation behaviors and volume changes.

36 MATERIALS SCIENCE↗

Development and Understanding of Nb 3 Sn films for radiofrequency applications through a sample-host 9-cell cavity

Nb 3 Sn is a promising advanced material under development for superconducting radiofrequency cavities. Past efforts have been focused primarily on small development-scale cavities, but large, often multi-celled cavities, are needed for particle accelerator applications. In this work, we report on successful Nb 3 Sn coatings on Nb in a 1 m-long 9-cell Nb sample-host cavity at Fermilab. The geometry of the first coating with only one Sn source made it possible to study the influence of Sn flux on the microstructure. Based on these results, we postulate a connection between recently observed anomalously large thin grains and uncovered niobium spots observed in the past by other authors (Trenikhina et al 2018 Supercond. Sci. Technol. 32 015004). A phenomenological model to explain how these anomalously large grains could form is proposed. Overall, this model is invoked to provide possible explanations for literature results from several groups and to guide key process parameters to achieve uniform vapor-diffusion coatings, when applied to complex structures as the multi-cell cavity under study.

43 PARTICLE ACCELERATORS↗