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At least 163 records · Page 9

Development of Coatings for Tantalum Alloy Nozzle Vanes

A group of silicide coatings developed for the T222 tantalum-base alloy have afforded over 600 hours of protection at 1600 and 2400 F during cyclic exposure in air. These coatings were applied in two steps. A modifier alloy was applied by slurry techniques and was sintered in vacuum prior to siliciding by pack cementation in argon. Application of the modifier alloy by pack cementation was found to be much less effective. The addition of titanium and vanadium to molybdenum and tungsten yielded beneficial modifier alloys, whereas the addition of chromium showed no improvement. After siliciding, the 15Ti- 35W-15V-35Mo modifier alloy exhibited the best performance; one sample survived 1064 hours of oxidation at 2400 F. This same coating was the only coating to reproducibly provide 600 hours of protection at both 1600 and 2400 F; in the second and third of three experiments, involving oxidation of three to five specimens at each temperature in each experiment, no failures were observed in 600 hours of testing. The slurry coatings were also shown to protect the Cb752 and D43 columbium-base alloys.

PROTECTIVE COATING↗

Evaluation of 10V Chip Polymer Tantalum Capacitors for Space Applications

Due to low ESR and safe failure mode, new technology chip polymer tantalum capacitors (CPTC) have gained popularity in the electronics design community, first in commercial applications, and now in hi-rel and space systems. The major drawbacks of these parts are high leakage currents, degradation under environmental stresses, and a relatively narrow temperature range of operating and storage conditions. Several studies have shown that a certain amount of moisture in polymer cathodes is necessary for a normal operation of the parts. This might limit applications of CPTCs in space systems and requires analysis of long-term exposure to deep vacuum conditions on their performance and reliability. High leakage currents and limited maximum operational temperature complicate accelerated testing that is necessary to assess long-term reliability and require new screening and qualification procedures for quality assurance. A better understanding of behavior of CPTCs as compared to traditional, MnO2, capacitors is necessary to develop adequate approaches for QA system for space applications. A specific of CPTCs is that different materials and processes might be used for low-voltage (10 V and less) and high-voltage (above 10 V) capacitors, so performance and degradation processes in these groups require separate analysis. In this work, that is a part of the NASA Electronic Parts and Packaging (NEPP) program, degradation of AC and DC characteristics under environmental stresses at different temperatures and voltages have been studied in nine lots of commercial and automotive grade capacitors rated to 10 V. Results of analysis of leakage currents, high temperature storage (HTS) up to 5000 hrs in vacuum and air at different temperatures, and Highly Accelerated Life Testing (HALT) in the range from 85 C to 145 C are presented. Temperature and voltage acceleration factors were calculated based on approximation of distributions of degradation rates with a general log-linear Weibull model. Mechanisms of degradation and failures, and requirements for screening and qualification testing are discussed.

Tantalum Capacitors↗

Degradation and ESR Failures in MnO2 Chip Tantalum Capacitors

Equivalent series resistance (ESR) of chip tantalum capacitors determines the rate of energy delivery and power dissipation thus affecting temperature and reliability of the parts. Employment of advanced capacitors with reduced ESR decreases power losses and improves efficiency in power systems. Stability of ESR is essential for correct operations of power units and might cause malfunctioning and failures when ESR becomes too high or too low. Several cases with ESR values in CWR29 capacitors exceeding the specified limit that were observed recently raised concerns regarding environmental factors affecting ESR and the adequacy of the existing screening and qualification testing. In this work, results of stress testing of various types of military and commercial capacitors obtained over years by GSFC test lab and NEPP projects that involved ESR measurements are described. Environmental stress tests include testing in humidity and vacuum chambers, temperature cycling, long-term storage at high temperatures, and various soldering simulation tests. Note that in many cases parts failed due to excessive leakage currents or reduced breakdown voltages. However, only ESR-related degradation and failures are discussed. Mechanisms of moisture effect are discussed and recommendations to improve screening and qualification system are suggested.

Equivalent Series Resistance (ESR)↗

Evaluation of Series T22 Wet Tantalum Capacitors

Several types of advanced wet tantalum capacitors, and series T22 in particular, are designed without internal Teflon sealing that is used for military grade, CLR style capacitors. This raises concerns regarding hermeticity of the single seal parts and their capability to withstand high internal gas pressures that might develop during operation in space. To address these issues, T22 series capacitors rated to 50 V and 125 V were subjected to highly accelerated life testing (HALT) at 125 C and rated voltage and step stress random vibration testing (RVT). To simulate conditions of storage or operation under increased internal gas pressure, the parts were stored at temperature of 150 C for 2500 hr (HTS150). Electrical characteristics of the parts were measured through the storage testing and the hermeticity leak rate was tested before and after HTS150. To assess thermo-mechanical robustness of the part, capacitors were manually soldered onto printed wired boards (PWB) and stressed by 1000 temperature cycles between -55 C and +125 C. The effect of temperature cycling was assessed by additional HALT at different temperatures. Results show that T22 series capacitors have robust design and can satisfy requirements for space applications.

Wet tantalum capacitors↗

Breakdown and Self-healing in Tantalum Capacitors

Reliability of tantalum capacitors depends on the efficiency of self-healing that restores parts after breakdown. In this work, different types of polymer and MnO2 cathode capacitors have been tested for scintillation breakdown using a constant current stress (CCS) technique modified to allow detection of amplitudes and duration of current spikes. Monitoring of leakage currents with time under bias is used to assess the effect of scintillations. The appearance and composition of damaged sites have been examined after deprocessing and cross-sectioning. Thermal processes during scintillations have been analyzed, a mechanism of breakdown based on growth of conductive filaments in the dielectric suggested, and self-healing processes in polymer and MnO2 cathode capacitors discussed.

tantalum capacitor↗

Metrics for Anomalous Charging currents in Polymer Tantalum Capacitors

Anomalous charging currents (ACC) in polymer tantalum capacitors may appear as a temporary short circuit that can last for dozens of milliseconds, cause failures to the parts, or cause malfunctions to fast operating electronic systems. Currently, there is no standard technique or set of metrics to evaluate the level of ACC which compares results obtained by different users and manufacturers. In this work, ACC in different types of capacitors were characterized by analysis of current transients during the constant voltage ramp or power surge testing (PST) techniques. It is shown that although the shape of transients may vary at different test conditions, the transfer charge and energy remain practically the same. The level of ACC is characterized by the energy dissipated in the part during PST. Variations of the dissipated energy with moisture content, test temperature, and voltage are evaluated. Effects of different reflow soldering conditions and long-term (up to 3000 hours) storage at 125 °C are discussed.

polymer tantalum capacitor↗

Experiments to Measure the Effect of Tantalum on Critical Systems

Sandia National Laboratories (SNL) and Oak Ridge National Laboratory (ORNL) collaborated to develop a capability to test the epithermal/intermediate cross sections of materials at the SNL critical experiment facility using the Seven Percent Critical Experiment (7uPCX) fuel. As a result, a new set of critical experiments has been designed to target the epithermal cross sections of tantalum (Ta) and is scheduled to be performed at SNL in 2023. These critical experiments will be evaluated for inclusion in the 2024 edition of the International Criticality Safety Benchmark Evaluation Project (ICSBEP) Handbook. The focus of these critical experiments is to measure the effects of Ta on the critical array size. The critical array size will be determined by an approach-to-critical experiment with the number of fuel rods in the array as a free parameter. The core configurations are designed to optimize the reactivity worth of Ta and the overall percentage of Ta absorption rates in the epithermal/intermediate energy range (0.625 eV – 100 keV). The baseline core configuration includes 7uPCX fuel rods set at a triangular pitch of 1.016 cm and a central dry test region that utilizes a cadmium liner for filtering out thermal neutrons. The central test region has locations for 85 Ta rods set at a triangular pitch of 0.813 cm. The Ta reactivity worth for the case with 85 Ta rods is approximately 2.55%, with the percentage of Ta absorption rates within the intermediate energy range at nearly 90%.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Nuclear Data Sensitivity/Uncertainty Studies of Tantalum-Reflected Systems

Tantalum (Ta) is a refractory metal with high melting point and high corrosion resistance. This makes it useful as a mold material for plutonium casting operations. Unfortunately, there are few criticality benchmarks with high nuclear data sensitivities. Given that, it is desirable to design new experiments to provide additional validation data for nuclear criticality safety, which is the objective of the Thales project. Multiple application models were used to represent process conditions (either normal conditions or credible upset conditions) both at Los Alamos National Laboratory (LANL) and Savannah River Site (SRS). A total of 40 application models were obtained. Given this, it was useful to down-select the number of needed application models. This work documents the down-selection based on several nuclear data sensitivity/uncertainty metrics. In addition to showing the result of the specific down-selection used for the Thales project, this work discusses potential ways to represent a large number of application models with a smaller number of proposed experiment designs.

42 ENGINEERING↗

Rapid Polyolefin Hydrogenolysis by a Single‐Site Organo‐Tantalum Catalyst on a Super‐Acidic Support: Structure and Mechanism

Abstract The novel electrophilic organo‐tantalum catalyst AlS/TaNp x ( 1 ) (Np=neopentyl) is prepared by chemisorption of the alkylidene Np 3 Ta=CH t Bu onto highly Brønsted acidic sulfated alumina (AlS). The proposed catalyst structure is supported by EXAFS, XANES, ICP, DRIFTS, elemental analysis, and SSNMR measurements and is in good agreement with DFT analysis. Catalyst 1 is highly effective for the hydrogenolysis of diverse linear and branched hydrocarbons, ranging from C2 to polyolefins. To the best of our knowledge, 1 exhibits one of the highest polyolefin hydrogenolysis activities (9,800 (CH 2 units) ⋅ mol(Ta) −1 ⋅ h −1 at 200 °C/17 atm H 2 ) reported to date in the peer‐reviewed literature. Unlike the AlS/ZrNp 2 analog, the Ta catalyst is more thermally stable and offers multiple potential C−C bond activation pathways. For hydrogenolysis, AlS/TaNp x is effective for a wide variety of pre‐ and post‐consumer polyolefin plastics and is not significantly deactivated by standard polyolefin additives at typical industrial concentrations.

Lai, Qingheng↗

Quantifying Pore Morphology in Spray-Formed Tantalum Using X-ray Micro-computed Tomography

In order to establish quantitative process–structure–property relationships in thermal spray coatings, a robust framework for defining (micro)structural characteristics is needed. Here, we present a quantitative characterization of the three-dimensional morphology of porosity in spray-formed tantalum samples based on high-resolution X-ray micro-computed tomography. Using synchrotron facilities, we acquired dozens of high-resolution scans, enabling a statistically meaningful comparison across multiple samples, different regions within samples, and spray processes. We quantify the spatial distribution, size, and topology of porous inclusions, with a significant focus on variability across samples and different spray processes (plasma and cold sprayed), as well as sensitivity to image segmentation and resolution. Based on a typical segmentation, we report porosities ranging from 0.9 to 1.7 pct for all samples tested, with significant sensitivity due to image segmentation resulting in estimates as low as 0.6 pct and as high as 4.8 pct. For the complex pore space morphology observed in these materials, we argue that a conventional analysis based on identifying individual pores is not well suited, and propose an alternative approach based on morphological metrics with a rich history in porous media literature, such as spatial correlations, local pore thickness, and scale-dependent sub-sampling. Spatial correlations indicate anisotropic splat structures, but only mildly anisotropic pores. Various measures of pore size show a wide distribution of sizes, ranging from sub-micron to 10-micron length scales. Scale-dependent variations in porosity suggest that representative volumes of several hundred microns are required for convergence of morphological metrics, with larger volumes for cold-spray materials. This work provides a robust quantitative basis for describing three-dimensional pore structure in thermal spray coatings.

36 MATERIALS SCIENCE↗