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At least 109 records · Page 6

Nanostructural features degrading the performance of superconducting radio frequency niobium cavities revealed by transmission electron microscopy and electron energy loss spectroscopy

Nanoscale defect structure within the magnetic penetration depth of ∼100 nm is key to the performance limitations of niobium superconducting radio frequency cavities. Using a unique combination of advanced thermometry during cavity RF measurements, and TEM structural and compositional characterization of the samples extracted from cavity walls, we discover the existence of nanoscale hydrides in electropolished cavities limited by the high field Q slope, and show the decreased hydride formation in the electropolished cavity after 120 °C baking. Furthermore, we demonstrate that adding 800 °C hydrogen degassing followed by light buffered chemical polishing restores the hydride formation to the pre-120 °C bake level. We also show absence of niobium oxides along the grain boundaries and the modifications of the surface oxide upon 120 °C bake.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Oxide dissolution and oxygen diffusion scenarios in niobium and implications on the Bean–Livingston barrier in superconducting cavities

We generalize a native Nb 2 O 5 dissolution model [G. Ciovati, Appl. Phys. Lett. 89, 022507 (2006)] to sequential overlayer dissolutions, multilayer dissolution, and realistic temperature profiles, which may be applicable to other materials. The model is applied to secondary ion mass spectrometry depth profile measurements for varying temperature profiles and two-step oxide dissolution in Nb and found to agree well. In the context of the Meissner screening response due to impurity profiles on the length scale of the London penetration depth, the shallow diffusion of O impurities results in a substantial decrease in the peak supercurrent density near the surface. In this framework, oxide dissolution and oxygen diffusion can account for a rise in peak supportable magnetic field in SRF cavities with baking time and a suppression after the optimal baking time is reached, in good agreement with peak-field baking temperatures and times as well as recent quench field measurements.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Outgassing measurements of bare and magnetite-coated low-carbon steel vacuum chambers

The outgassing properties of bare and magnetite-coated AISI 1020 low-carbon steel vacuum chambers were evaluated to establish material selection criteria for extreme high vacuum applications, namely, to explore the possibility of using these materials to build next-generation spin-polarized photoelectron guns. Water outgassing measurements using the throughput method revealed that the magnetite-coated chamber exhibited five times lower outgassing at room temperature prior to baking, but this advantage disappears after 80 °C baking. Hydrogen outgassing measurements demonstrated significant differences after intensive heat treatment: the bare low-carbon steel vacuum chamber achieved a specific outgassing rate of 9.6 × 10 −16 Torr L s −1 cm −2 after 400 °C/50 h bake plus additional heat treatment at lower temperatures, 25 times lower than the magnetite-coated low-carbon steel chamber. Residual gas analysis showed >99% hydrogen composition after heat treatment for both materials, with carbon species below detection limits for bare low-carbon steel versus 0.8% for magnetite-coated surfaces. These measurements indicate that properly conditioned bare low-carbon steel can achieve the <10 −12 Torr pressures required for next-generation spin-polarized photogun applications. In conclusion, the paper includes various analysis techniques intended to explain observed behaviors: isotherm analysis of pump-down plots, Arrhenius analysis of hydrogen outgassing rate data, and residual gas composition tracking.

Adsorption isotherm↗

Hybrid chemical characterization of latent images in EUV resist with 12 nm half-pitch features

With the advancement of high numerical aperture extreme ultraviolet (EUV) lithography, the new platform will enable chipmakers to achieve critical dimensions of 8 nm. However, resist materials face significant challenges in delivering increased sensitivity while managing rising stochastic variations. We aim to develop comprehensive techniques to characterize the chemical profile of latent images, stored in EUV resists after exposure and postexposure baking, which is essential for understanding the origin of stochastic effects. Infrared photo-induced force microscopy (IR PiFM) is a bimodal atomic force microscopy technique combined with an infrared light source, allowing for simultaneous sub-5 nm topographic and chemical characterization within a localized environment. Critical-dimension resonant soft X-ray scatterometry (CD-RSoXS) provides statistical data that reveal structural and chemical information for comparative analysis. For the first time, IR PiFM has been used to chemically map the latent images of EUV resists (after exposure and postexposure baking) at a record high resolution of 12 nm half-pitch, enabling nondestructive analysis of patterns prior to development. Furthermore, CD-RSoXS offers direct experimental observation and comparison of exposed, postexposure baked, and developed patterns, which align with the IR PiFM results. We demonstrate that the IR PiFM technique offers valuable insights into both high spatial resolution and local chemical information simultaneously. In addition, CD-RSoXS provides statistical results that support our main findings. This hybrid metrology approach leverages a multifaceted dataset by combining the most reliable information from each source, which is essential for a comprehensive understanding of the stochastic effects in EUV lithography processes.

O’Reilly, Padraic↗

Thermal characterization and model free kinetics of aged epoxies and foams using TGA and DSC methods.

Two classes of materials, poly(methylene diphenyl diisocyanate) or PMDI foam, and cross-linked epoxy resins, were characterized using thermal gravimetric analysis (TGA) and differential scanning calorimetry (DSC), to help understand the effects of aging and %E2%80%9Cbake-out%E2%80%9D. The materials were evaluated for mass loss and the onset of decomposition. In some experiments, volatile materials released during heating were analyzed via mass spectroscopy. In all, over twenty materials were evaluated to compare the mass loss and onset temperature for decomposition. Model free kinetic (MFK) measurements, acquired using variable heating rate TGA experiments, were used to calculate the apparent activation energy of thermal decomposition. From these compiled data the effects of aging, bake-out, and sample history on the thermal stability of materials were compared. No significant differences between aged and unaged materials were detected. Bake-out did slightly affect the onset temperature of decomposition but only at the highest bake-out temperatures. Finally, some recommendations for future handling are made.

Cordaro, Joseph Gabriel↗

Corrosion Control in Carbon Fiber Reinforced Plastic (CFRP) Composite-Aluminum Closure Panel Hem Joints

This project targeted the implementation of CFRP/Al closure panels as a drop-in replacement for all-aluminum closures used in automobile production today. The project focused on the development of corrosion fundamentals involving CFRP materials and the use of those materials in mixed-material joints. Numerous studies were completed to benchmark current materials and test mixed metal joints. Good correlation was found between outdoor exposures and laboratory cyclic corrosion testing. The insights from the corrosion testing fundamentals and benchmarking phases informed the development of low-cure adhesive and electrocoats and conductive primers for the CFRP. Adhesive and electrocoat materials were successfully developed meeting low-cure targets for bake (150C/10min). These materials were scaled-up and used to produce 5 prototype liftgates to further evaluate CFRP/Al joints in a full-scale part. The lower cure materials enabled mitigation of CTE mismatch and reduced the required bake temperature, resulting in reduced part distortion. Corrosion testing of the liftgates revealed unexpected increases in corrosion relative to the standard bake materials. While rigorous evaluation of the parts was not possible due to numerous complexities associated with prototype testing, the results provided significant insights into the material behavior of CFRP/Al joints. Key learnings from the project included a better understanding of the system complexity (interplay of substrate/primer conductivity, production of full-scale prototypes), advances in coating/adhesive design for low-cure applications involving CFRP, and advancement of corrosion test protocols for CFRP.

36 MATERIALS SCIENCE↗

Decoupling of Nitrogen and Oxygen Impurities in Nitrogen Doped SRF Cavities

The performance of superconducting radiofrequency (SRF) cavities is critical to enabling the next generation of efficient high-energy particle accelerators. Recent developments have focused on altering the surface impurity profile through \textit{in-situ} baking, furnace baking, and doping to introduce and diffuse beneficial impurities such as nitrogen, oxygen, and carbon. However, the precise role and properties of each impurity are not well understood. In this work, we attempt to disentangle the role of nitrogen and oxygen impurities through time-of-flight secondary ion mass spectrometry of niobium samples baked at temperatures varying from 75-800 $^\circ$C with and without nitrogen injection. From these results, we developed treatments recipe that decouple the effects of oxygen and nitrogen in doping treatments. Understanding how these impurities and their underlying mechanisms drive further optimization in the tailoring of impurity profiles for high-performance SRF cavities.

43 PARTICLE ACCELERATORS↗

Oxide dissolution and oxygen diffusion scenarios in niobium and implications on the Bean–Livingston barrier in superconducting cavities

We generalize a native Nb2O5 dissolution model [G. Ciovati, Appl. Phys. Lett. 89, 022507 (2006)] to sequential overlayer dissolutions, multilayer dissolution, and realistic temperature profiles, which may be applicable to other materials. The model is applied to secondary ion mass spectrometry depth profile measurements for varying temperature profiles and two-step oxide dissolution in Nb and found to agree well. In the context of the Meissner screening response due to impurity profiles on the length scale of the London penetration depth, the shallow diffusion of O impurities results in a substantial decrease in the peak supercurrent density near the surface. In this framework, oxide dissolution and oxygen diffusion can account for a rise in peak supportable magnetic field in SRF cavities with baking time and a suppression after the optimal baking time is reached, in good agreement with peak-field baking temperatures and times as well as recent quench field measurements.

Lechner, Eric↗

Ultra-High Vacuum Outgassing Characterization of Thermally Processed Low-Carbon Steel for Advanced Particle Accelerator and Gravitational Wave Detector Applications

This dissertation investigated AISI 1020 low-carbon steel as an alternative vacuum chamber material to conventional stainless steel for ultra-high vacuum (UHV) and extreme-high vacuum (XHV) applications. After a 400 °C/48 h bake, AISI 1020 tube chambers achieved a hydrogen outgassing rate of 2.4 × 10¿¹6 Torr·L·s¿¹·cm¿², approximately 2,300 times lower than the prebaked 316L stainless-steel comparator, among the lowest hydrogen outgassing rates ever reported for an uncoated metallic vacuum chamber. Bare and magnetite-coated AISI 1020 chambers were then compared using throughput and rate-of-rise methods. The magnetite coating yielded 5× lower water outgassing at room temperature, but this advantage disappeared after 80 °C baking. After full thermal conditioning (400 °C/48 h prebake followed by 150 °C/96 h and 200 °C/110 h), bare steel achieved 25× lower hydrogen outgassing than the magnetite-coated chamber (9.6 × 10¿¹6 Torr·L·s¿¹·cm¿²) and >99% H2 purity with carbon species below RGA detection. Monte Carlo molecular flow simulations of a CEBAF photogun beamline (96 scenarios) showed that replacing 304L stainless steel with AISI 1020 reduces equilibrium H2 pressure by a factor of 833; a single 304L electrode contributes 98.8% of the gas load despite occupying only 9.1% of the internal surface area. A 500-m Einstein Telescope beampipe screening showed that corrugated bellows contribute 18% of the gas load from only 0.7% of the surface area. A five-model adsorption isotherm framework applied to 22 pumpdown datasets (164 fits with AR(1)-GLS correction) established that the experimental protocol, not the material, controls isotherm identifiability: Dubinin–Radushkevich wins isothermal pipe pumpdowns; Langmuir wins thermally dominated chamber bakes. Cross-dataset joint fitting of the AISI 1020 pipe pumpdowns yielded an H2 diffusion activation energy Ed = 7.24 ± 1.28 kcal·mol¿¹, consistent with trap dominated diffusion in commercial low-carbon steels. Two companion innovations were developed: a Variable Conductance Device (VCD, patent pending IDF-00723) for XHV outgassing measurement, and VacuumDesignerPro (VDP), a MATLAB-based design tool validated against LIGO benchmarks.

Al-Allaq, Aiman H [Old Dominion University]↗

Improved Bakeout Chambers Within Vacuum Chambers

Improved bakeout chamber incorporates hardware features that, in conjunction with improved bakeout procedure, reduce spurious contamination and increase accuracy of contamination measurements. When operated according to revised bakeout procedure, they yield measurements of contamination on vacuum-bake test articles more accurate than available previously, and potential for post-bake recontamination of vacuum-baked articles reduced. These chambers improved versions of one described in "Bakeout Chamber Within Vacuum Chamber" (NPO-18959). By enclosing test article in enclave and keeping walls of enclave hotter than test article during bakeout, one prevents condensation of contaminants on inner walls of enclave.

Johnson, Kenneth R.↗

Carbon XANES Data from Six Aerogel Picokeystones Cut from the Top and Bottom Sides of the Stardust Comet Sample Tray

Great care and a large effort was made to minimize the amount of organic matter contained within the flight aerogel used to collect Comet 81P/Wild 2 samples. Even so, by the very nature of the production process and silica aerogel s affinity for volatile organics keeping silica aerogel free from organics is a monumental task. Silica aerogel from three production batches was flown on the Stardust sample return mission. All 3 types had layered densities varying from 5mg/ml to 50 mg/ml where the densest aerogel was farthest away from the collection area. A 2 step gelation process was used to make the flight aerogel and organics used in this process were tetraethylorthosilicate, ethanol and acetonitrile. Both ammonium hydroxide and nitric acid were also used in the aerogel production process. The flight aerogel was baked at JPL at 300 C for 72 hours, most of the baking was done at atmosphere but twice a day the oven was pumped to 10 torr for hour [1]. After the aerogel was baked it was stored in a nitrogen purged cabinet until flight time. One aerogel cell was located in the SRC away from any sample collection area as a witness to possible contamination from out gassing of the space craft, re-entry gases and any other organic encounter. This aerogel was aerogel used in the interstellar collection sample tray and is the least dense of the 3 batches of aerogel flown. Organics found in the witness tile include organics containing Si-CH3 bonds, amines and PAHS. Besides organic contamination, hot spots of calcium were reported in the flight aerogel. Carbonates have been detected in comet 81P/Wild2 samples . During preflight analyses, no technique was used to analyze for carbonates in aerogel. To determine if the carbonates found in 81P/Wild2 samples were from the comet, it is necessary to analyze the flight aerogel for carbonate as well as for organics.

Wirick, S.↗

Effect of Preconditioning and Soldering on Failures of Chip Tantalum Capacitors

Soldering of molded case tantalum capacitors can result in damage to Ta205 dielectric and first turn-on failures due to thermo-mechanical stresses caused by CTE mismatch between materials used in the capacitors. It is also known that presence of moisture might cause damage to plastic cases due to the pop-corning effect. However, there are only scarce literature data on the effect of moisture content on the probability of post-soldering electrical failures. In this work, that is based on a case history, different groups of similar types of CWR tantalum capacitors from two lots were prepared for soldering by bake, moisture saturation, and longterm storage at room conditions. Results of the testing showed that both factors: initial quality of the lot, and preconditioning affect the probability of failures. Baking before soldering was shown to be effective to prevent failures even in lots susceptible to pop-corning damage. Mechanism of failures is discussed and recommendations for pre-soldering bake are suggested based on analysis of moisture characteristics of materials used in the capacitors' design.

multilayer ceramic capacitor (MLCC)↗

CONTAMINATION CONTROL FOR ULTRA-SENSITIVE LIFE DETECTION SCIENCE MISSIONS

"This study report summarizes technological developments in science-required contamination control for cost-capped, life-detection missions in the Solar System. Technology advances focus on developing implementable strategies to restrict contamination of the spacecraft and instruments by the launch vehicle hardware. Secondary bake out operations during cruise further reduce molecular contaminants down to femtomolar levels in the sample path. The study validated a full-spacecraft, deployable barrier design as an effective strategy to isolate the spacecraft from the pre-launch processing and launch environment (e.g., fairing acoustic materials). It accommodates late mounting of RTGs and other required prelaunch activities. A new, high-fidelity physics, contamination-transport model for particles (including cells and their parts) and science-relevant molecules (e.g., possible biomolecules) was developed to validate the barrier concept. Importantly, this model takes into account the physics of extremely clean surfaces achieved by the best traditional contamination engineering. The ability to deal with very low levels of particulate and molecular contamination makes this model unique among standard contamination modeling approaches. Modeling also demonstrated that a high-temperature bake out during interplanetary cruise of the sample collector that comprises the largest surface area in the sample path for an Enceladus orbiter reference mission, was extremely effective. This study included the evaluation of other details necessary for an effective contamination control strategy for life detection missions including feasibility of achieving parts per trillion level cleanliness for semi-volatile hydrocarbons in nitrogen purge gas, identification of launch vehicle services required for the baseline contamination control, and defining additional contamination control measures to be taken during launch operations. Key results of the study are: • New spacecraft barrier design that accommodates RTGs is readily cleanable and repairable. Deployment of a 1/3 scale model was successfully demonstrated. • The barrier reduces particle contamination (likely biological) from fairing to spacecraft by 1e-2 to 1e-3. • On-cruise bake-out of critical surfaces significantly reduced molecular contamination (by as much as 1e-12). Subsequently, the probability of a surface contamination particle being transported to an instrument by an ice particle is less than 5.1e-5 (for microbes specifically, 4.39e-10). The report concludes that a full-spacecraft barrier designed specifically for life-detection missions that require stringent control of particulate and molecular contaminates is an effective means of mitigating risks of false positive and negative results for life signature investigations. Further, secondary cleaning steps for critical sections of the sample path can be highly effective at reducing molecular contaminants to low femtomolar levels."

Contamination↗

Contamination Control for Ultra-Sensitive Life-Detection Missions

"This study report summarizes technological developments in science-required contamination control for cost-capped, life-detection missions in the Solar System. Technology advances focus on developing implementable strategies to restrict contamination of the spacecraft and instruments by the launch vehicle hardware. Secondary bake out operations during cruise further reduce molecular contaminants down to femtomolar levels in the sample path. The study validated a full-spacecraft, deployable barrier design as an effective strategy to isolate the spacecraft from the pre-launch processing and launch environment (e.g., fairing acoustic materials). It accommodates late mounting of RTGs and other required prelaunch activities. A new, high-fidelity physics, contamination-transport model for particles (including cells and their parts) and science-relevant molecules (e.g., possible biomolecules) was developed to validate the barrier concept. Importantly, this model takes into account the physics of extremely clean surfaces achieved by the best traditional contamination engineering. The ability to deal with very low levels of particulate and molecular contamination makes this model unique among standard contamination modeling approaches. Modeling also demonstrated that a high-temperature bake out during interplanetary cruise of the sample collector that comprises the largest surface area in the sample path for an Enceladus orbiter reference mission, was extremely effective. This study included the evaluation of other details necessary for an effective contamination control strategy for life detection missions including feasibility of achieving parts per trillion level cleanliness for semi-volatile hydrocarbons in nitrogen purge gas, identification of launch vehicle services required for the baseline contamination control, and defining additional contamination control measures to be taken during launch operations. Key results of the study are: • New spacecraft barrier design that accommodates RTGs is readily cleanable and repairable. Deployment of a 1/3 scale model was successfully demonstrated. • The barrier reduces particle contamination (likely biological) from fairing to spacecraft by 1e-2 to 1e-3. • On-cruise bake-out of critical surfaces significantly reduced molecular contamination (by as much as 1e-12). Subsequently, the probability of a surface contamination particle being transported to an instrument by an ice particle is less than 5.1e-5 (for microbes specifically, 4.39e-10). The report concludes that a full-spacecraft barrier designed specifically for life-detection missions that require stringent control of particulate and molecular contaminates is an effective means of mitigating risks of false positive and negative results for life signature investigations. Further, secondary cleaning steps for critical sections of the sample path can be highly effective at reducing molecular contaminants to low femtomolar levels."

contamination, life detection, barrier, modeling↗

Water and Ammonia Desorption from 5A Zeolite

The objective of this project is to demonstrate the adsorption and desorption characteristics of water and ammonia on 5A zeolite during regeneration conditions. As discussed in literature, zeolite material is a crystalline hydrated aluminosilicate material. Zeolites have high cation exchange ability and are commonly used as adsorbents in separation and purification processes. The property of uniformly sized pores allows zeolites to selectively separate gases. Because they have varying ion selectivity, there is competitive adsorption in a multicomponent mixture. 5A zeolite has a uniform pore diameter of 5 Angstroms. Water and ammonia are miscible components with similar molecular weights and size. This makes distinguishing the two compounds difficult using mass spectrometry. In a previous study, it was shown that water tends to desorb from 5A zeolite from 40 deg. C to 353 deg. C with peaks at 177 deg. C and 244 deg. C, while ammonia tends to desorb from 300 deg. C to 580 deg. C with a peak at 436 deg. C as determined using a Micromeritics AutoChem 2920 Instrument. The one drawback of using a Micromeritics Instrument is that only a few milligrams of sample material can be used. Bench scale tests can better demonstrate desorption characteristics of water and ammonia during regeneration from 5A zeolite material. Water in argon carrier gas and ammonia in hydrogen carrier gas will be tested separately, then a mixture of the two will be tested. Initial bake-out conditions: hydrogen carrier gas, slowly raise temp to approximately 450 deg. C until desired moisture content <100 ppm is achieved. Water loading: argon carrier gas through bubbler until breach is observed using the residual gas analyzer (RGA). Ammonia loading: hydrogen carrier gas through system until breach is observed using RGA. Regeneration conditions: hydrogen carrier gas, raise temp to approximately 300 deg. C, then slowly to 450 deg. C. Observe signals on RGA. Weigh samples between tests and integrate RGA signals. Accomplishments: Developed work control documentation and completed safety related requirements; Flow sheet and test system development; Initial bake-out of first sample. Testing will determine if regenerating zeolite material can be safely accomplished by high-temperature bake-out to remove ammonia. If unsuccessful, ammonia would only be removed at the end of life.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Decoupling of Nitrogen and Oxygen Impurities in Nitrogen Doped SRF Cavities

The performance of superconducting radiofrequency (SRF) cavities is critical for enabling the next generation of efficient high-energy particle accelerators. Recent developments have focused on altering the surface impurity profile through \textit{in-situ} baking, furnace baking, and doping to introduce and diffuse beneficial impurities such as nitrogen, oxygen, and carbon. However, the precise role and properties of each impurity are not well understood. In this work, we attempt to disentangle the role of nitrogen and oxygen impurities through time-of-flight secondary ion mass spectrometry using niobium cavity cutouts baked at temperatures varying from 120-800$^\circ$C with and without nitrogen injection. Understanding the underlying mechanisms behind these impurities will drive further optimization in the tailoring of nitrogen and oxygen profiles for high-performance SRF cavities.

43 PARTICLE ACCELERATORS↗

Controlling Oxidation of Nb in Oxygen Abundant Environments.

Superconducting Radio Frequency (SRF) cavities, the core of modern particle accelerators, rely on high-purity niobium (Nb) to achieve high quality factors and accelerating gradients. However, native oxidation in ambient conditions introduces a complex oxide layer with increased surface defects and contamination, particularly from carbon. This research explores a controlled oxidation processes in an oxygen-abundant environment to try to control this complex oxide stack, with the goal of improving surface purity and uniformity. Using standard surface preparation techniques—including electropolishing, vacuum baking, and sonication—followed by a custom oxidation protocol, we compared structural and chemical changes through Confocal Microscopy, Scanning Electron Microscopy (SEM), and X-Ray Photoelectron Spectroscopy (XPS). Results show that iterative oxidation cycles can significantly reduce carbon-related defects, even without baking. Aditionally, baked samples with a specific oxidation technique demonstrated a measurable 25\% decrease in carbide formation.

Romero, Juan [Fermilab]↗

Poly(methyl methacrylate) as a self-assembled gate dielectric for graphene field-effect transistors

We investigate poly(methyl methacrylate) (PMMA) as a low thermal budget organic gate dielectric for graphene field effect-transistors (GFETs) based on a simple process flow. We show that high temperature baking steps above the glass transition temperature (∼130 °C) can leave a self-assembled, thin PMMA film on graphene, where we get a gate dielectric almost for “free” without additional atomic layer deposition type steps. Electrical characterization of GFETs with PMMA as a gate dielectric yields a dielectric constant of k = 3.0. GFETs with thinner PMMA dielectrics have a lower dielectric constant due to decreased polarization arising from neutralization of dipoles and charged carriers as baking temperatures increase. The leakage through PMMA gate dielectric increases with decreasing dielectric thickness and increasing electric field. Unlike conventional high-k gate dielectrics, such low-k organic gate dielectrics are potentially attractive for devices such as the proposed Bilayer pseudoSpin Field-Effect Transistor or flexible high speed graphene electronics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗