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At least 1,531 records · Page 85

Focused Ion Beam Preparation of Low Melting Point Metals: Lessons Learned From Indium

Indium (In) and other low melting point metals are used as interconnects in a variety of hybridized circuits and a full understanding of the metallurgy of these interconnects is important to the reliability and performance of the devices. Here, this paper shows that room temperature focused ion beam (FIB) preparation of cross-sections, using Ga + or Xe + can result in artifacts that obscure the true In microbump structure. The use of modified milling strategies to minimize the increased local sample temperature are shown to produce cross-sections that are representative of the In bump microstructure in some sample configurations. Furthermore, cooling of the sample to cryogenic temperatures is shown to reliably eliminate artifacts in FIB prepared cross-sections of In bumps allowing the true bump microstructure to be observed.

36 MATERIALS SCIENCE↗

Quantitation of Trace Water in ISS Atmosphere Samples Recovered from CO2-Removal Systems

As crewed spaceflight continues to push the limits of exploration, instruments and hardware used to maintain and monitor crew and vehicle health, must become more integrated, reliable, and efficient. By combining a carbon dioxide (CO2) removal system with a resource recovery system like a Sabatier or Bosch reactor, the waste gas from the removal system can be converted into valuable resources that help reduce reliance on ground resupply. Due to the high-pressure nature of the Sabatier and Bosch reactions, the vent gas from most CO2 removal systems will need to be compressed before it can be processed. In order to prevent condensation in the compressor of the recovery system, it is critical to ensure that the vent stream from the CO2 removal system does not contain an excess of water. There are currently two different CO2 removal systems that are being developed as candidates for exploration missions. Each of these systems will be evaluated as a technology demonstration on ISS, and vent gas samples will be collected in Summa sampling canisters fitted with Entech valves for ground analysis. Due to the need to measure low levels of water in these samples, it was not possible to use the current ISS mini-grab sample containers (m-GSC) to collect these samples. The Summa containers, which were used to collect archive samples during Shuttle missions, have a different surface treatment that makes it possible to measure the low levels of water in samples collected in these containers. This paper will provide some background on the CO2 removal systems being evaluated for exploration missions as well as results from ground-based testing of the Summa canisters. Details on the development of the analytical method and the plan for preparing the canisters that will be used for in-flight sampling are also discussed.

William M. King↗

Tank 14H Preliminary Cease Waste Removal Sample Analyses

Savannah River Mission Completion Waste Removal and Tank Closure requested that Savannah River National Laboratory perform characterization analyses of Tank 14H in support of closure activities, specifically preliminary cease waste removal. This report provides important characterization of the prepared filtrate and air-dried solids in the January 2026 Tank 14H sample, HTF-14-26-1,2,3,4,5,6, for I-129, Tc-99, Cs-137, and Sr-90. The results reported here were utilized by SRMC to declare preliminary cease waste removal for Tank 14H.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Surface film effects on drop tube undercooling studies

The effects of various gaseous atmospheric constituents on drop-tube solidified samples of elemental metals were examined from a microstructural standpoint. All specimens were prepared from the purest available elements, so effects of impurities should not account for the observed effects. The drop-tube gas has a definite effect on the sample microstructure. Most dramatically, the sample cooling rate is effected. Some samples receive sufficient cooling to solidify in free fall while others do not, splating at the end of the drop tube in the sample catcher. Gases are selectively absorbed into the sample. Upon solidification gas can become less soluble and as a result forms voids within the sample. The general oxidation/reduction characteristics of the gas also affect sample microstructures. In general, under the more favorable experimental conditions including reducing atmospheric conditions and superheatings, examination of sample microstructures indicates that nucleation has been suppressed. This is indicated by underlying uniform dendrite spacings throughout the sample and with a single dendrite orientation through most of the sample. The samples were annealed yielding a few large grains and single or bi-crystal samples were commonly formed. This was especially true of samples that were inadvertently greatly superheated. This is in contrast with results from a previous study in which surface oxides were stable and contained numerous sites of nucleation. The number of nucleation events depends upon the surface state of the specimen as determined by the atmosphere and is consistent with theoretical expectations based upon the thermodynamic stability of surface oxide films. Oxide-free specimens are characterized by shiny surfaces, with no observable features under the scanning electron microscope at 5000X.

Ethridge, E. C.↗

Materials preparation, single-crystal growth, and the phase diagram of the cuprate high-temperature superconductor La 1.6-x Nd 0.4 Sr x CuO 4

One branch of the La-214 family of cuprate superconductors, La 1.6-x Nd 0.4 Sr x CuO 4 (NdLSCO), has been of significant and sustained interest, in large part because it displays the full complexity of the phase diagram for canonical hole-doped, high TC superconductivity, while also displaying relatively low superconducting critical temperatures. The low superconducting TC’s imply that experimentally accessible magnetic fields can suppress the superconductivity to zero temperature. In particular, this has enabled various transport and thermodynamic studies of the T = 0 ground state in Nd-LSCO, free of superconductivity, across the critical doping p* = 0.23 where the pseudogap phase ends. The strong dependence of its superconducting properties on its crystal symmetry has itself motivated careful studies of the Nd-LSCO structural phase diagram. This paper provides a systematic study and summary of the materials preparation and characterization of both single crystal and polycrystalline samples of Nd-LSCO. Single-phase polycrystalline samples with x spanning the range from 0.01 to 0.40 have been synthesized, and large single crystals of La 1.6-x Nd 0.4 Sr x CuO 4 for select x across the region (0.07, 0.12, 0.17, 0.19, 0.225, 0.24, and 0.26) were grown by the optical floating zone method. Furthermore, systematic neutron and X-ray diffraction studies on these samples were performed at both low and room temperatures, 10 K and 300 K, respectively. These studies allowed us to follow the various structural phase transitions and propose an updated structural phase diagram for NdLSCO. In particular, we found that the low-temperature tetragonal (LTT) phase ends at a critical doping p LTT = 0.255±0.005, clearly separated from p*.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

A scanning quantum cryogenic atom microscope at 6 K

The Scanning Quantum Cryogenic Atom Microscope (SQCRAMscope) is a quantum sensor in which a quasi-1D quantum gas images electromagnetic fields emitted from a nearby sample. We report improvements to the microscope. Cryogen usage is reduced by replacing the liquid cryostat with a closed-cycle system and modified cold finger, and cryogenic cooling is enhanced by adding a radiation shield. The minimum accessible sample temperature is reduced from 35~K to 5.7~K while maintaining low sample vibrations. A new sample mount is easier to exchange, and quantum gas preparation is streamlined.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

2019 accomplishments: degradation of mechanical properties in structural metals and welds for FTS reservoirs

This report documents work in 2019 at SRNL in support of the Aging and Lifetimes program. Specimens for fracture toughness testing were prepared in prior years by thermally pre-charging samples, provided by Sandia National Laboratories, of welded types 304L and 21-6-9 stainless steels. These samples were pre-charged in 2017. The fracture toughness of the first aged specimens was measured and compared to historical data. The measurements of the 304L and 21-6-9 weld and particularly HAZ represent some of the first fracture data relevant to modern GTS reservoirs. This work represents an on-going collaboration between SRNL and SNL to understand tritium embrittlement of structural metals in Gas Transfer System reservoirs which informs lifetime assessments. Continued testing was conducted on ongoing historical studies, including the effects of very long-term aging, and the relative performance of differently forged stockpile relevant 304L and 316L samples. New samples were pre-charged with tritium and placed in a freezer for an aging study to allow helium to build into the material. The precharged samples consist of smooth and notched tensile samples of 304L stainless steel, as well as tube tensile samples of different thermal treatments supplied by Sandia National Laboratories. Their charging marks the beginning of a new sequence of studies to explore fundamental deformation mechanisms underpinning tritium embrittlement. At predesignated times, samples will be removed from aging and tested to provide data which will help develop an understanding of material degradation with increasing aging time. Also documented is progress in employing various advanced characterization techniques including high resolution electron microscopy, thermally programed desorption, and small angle x-ray scattering, as well as facilities renovations and equipment procurements in support of sustained tritium impacts on materials program at SRNL.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

200-IA-1 Operable Unit Human Health Risk and Kd Screen

The purpose of this environmental calculation file (ECF) is to provide the following: Document the data processing and data reduction steps taken to prepare the 200-IA-1 Operable Unit (OU) data set that will be used to calculate the sample-specific screening level human health risk evaluation; Document the data processing and data reduction steps taken to prepare the 200-IA-1 OU data set that will be used to identify analytes that could potentially impact groundwater in the future beneath the 200-IA-1 OU representative waste sites; Document the assumptions, equations, and methodologies used to calculate the screening levels for human health cancer risks and noncancer hazards for each representative waste site assigned to the 200-IA-1 OU. Individual measured soil concentrations from 0 to 4.6 m (15 ft) below ground surface (bgs) (shallow vadose zone) are used to calculate the total excess lifetime cancer risk (ELCR) and hazard index (HI) for the outdoor worker scenario to determine if there is a basis for remedial action. Individual measured soil concentrations from the ground surface to the groundwater table are used for the distribution coefficient (Kd) screen to identify analytes that could potentially impact groundwater in the future beneath the 200-IA-1 OU representative waste sites. This ECF supports DOE/RL-2020-51, 200-IA-1 OU Focused Feasibility Study, under the Comprehensive Environmental Response, Compensation, and Liability Act of 1980 (CERCLA). A risk characterization based upon the evaluation of the health risk estimates developed in this ECF will be presented in the focused feasibility study report.

63 RADIATION, THERMAL, AND OTHER ENVIRON. POLLUTAN↗

Rhodotorula toruloides Nitrogen Limitation PTM Profiling Multi-Omics (TZ-DP1).

The purpose of this experiment was to evaluate the regulatory stress response of Oleaginous yeast species Rhodotorula toruloides NBRC 0880 (JGI strain IFFO0880 v4.0) under nitrogen-rich and nitrogen-limited conditions over time. Time course experimental samples (24, 48, and 72 hours after inoculation) were prepared using a semi-automated multi-PTM proteomic approach, using tandem mass tag 18-plex (TMT18), and lipidome remodeling for downstream multi-omics analysis.

59 BASIC BIOLOGICAL SCIENCES↗

Metal-wool heat shields for space shuttle

The packaging of metal wool for reusable thermal heat shields applied to aerodynamic and other surfaces for the space shuttle was analyzed and designed, and samples were fabricated and experimentally studied. Parametric trends were prepared for selected configurations. An all-metal thermally efficient, reliable, reusable and producible heat shield system was designed and structurally tested for use on spacecraft aerodynamic surfaces where temperatures do not exceed 810 K. Stainless steel sheet, primarily for structure and secondarily in the transverse plane for thermal expansion, was shown to accommodate thermal expansion in all directions when restrained at the edges and heated to 1360 K. Aerodynamic loads of 0.35 x 1000,000 newtons/sq meter, and higher, may be easily accepted by structures of this design. Seven all-metal thermal protection specimens, 12.7 cm square and 2.5 cm thick were fabricated and are being experimentally evaluated at simulated shuttle entry conditions in an arc jet facility.

Miller, R. C.↗

Non-noble catalysts and catalyst supports for phosphoric acid fuel cells

Tungsten carbide, which is known to be active for hydrogen oxidation and CO tolerant has a hexagonal structure. Titanium carbide is inactive and has a cubic structure. Four different samples of the cubic alloys Wx-1TixC were prepared and found to be active and CO tolerant. These alloys are of interest as possible phosphoric acid fuel cell catalysts. They also are of interest as opportunities to study the activity of W in a different crystalline environment and to correlate the activities of the surface sites with surface composition.

Mcalister, A. J.↗

Changes in spectral properties of detached leaves

If leaf senescence can be delayed for several days without significant changes in spectral properties, then samples of leaves at remote test sites could be prepared and shipped to laboratories to measure spectral properties. The changes in spectral properties of detached leaves were determined. Leaves from red birch and red pine were immersed in water or 0.001 M benzylaminopurine (BAP) and stored in plastic bags in the dark at either 5 or 25 C. Total directional-hemispherical reflectance and transmittance of the adaxial surface of birch leaves were measured over the 400 to 1100 nm wavelength region with a spectroradiometer and integrating sphere. Pine needles were taped together and reflectance of the mat of needles was measured. Spectral properties changed less than 5% of initial values during the first week when leaves were stored at 5 C. Storage at 25 C promoted rapid senescence and large changes in spectral properties. BAP delayed, but did not stop, senescence at 25 C.

Daughtry, C. S. T.↗

Synthesis of polycrystalline chalcopyrite semiconductors by microwave irradiation

Polycrystalline samples of the chalcopyrites CuInS2, CuInSe2, and CuInSSe were prepared from stoichiometric mixtures of the pure elements by microwave irradiation. The reactions were performed in sealed quartz tubes in as few as 3 minutes. The products were analyzed by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray analysis, and X-ray photoelectron spectroscopy. The surface morphology and shape of the particles produced by this method suggest that the products are formed from liquid melts. This method could be applied to the production of bulk chalcopyrite as sources for thin film growth.

Landry, Christopher C.↗

STS-87 Day 14 Highlights

On this fourteenth day of the STS-87 mission, the flight crew, Cmdr. Kevin R. Kregel, Pilot Steven W. Lindsey, Mission Specialists Winston E. Scott, Kalpana Chawla, and Takao Doi, and Payload Specialist Leonid K. Kadenyuk focus on completion of hands-on sample processing in the microgravity glovebox facility. They also prepare the spacesuits and tools that will be used for the EVA by Scott and Doi. The crew take time out from their schedule to discuss the mission with reporters from the U.S., Japan and the Ukraine during the traditional in-flight news conference.

Source record↗

Vapor Grown Carbon Fiber/Phenolic Matrix Composites for Rocket Nozzles and Heat Shields

The ablation and mechanical and thermal properties of vapor grown carbon fiber (VGCF)/phenolic resin composites were evaluated to determine the potential of using this material in solid rocket motor nozzles. Composite specimens with varying VGCF loading (30%-50% wt) including one sample with ex-rayon carbon fiber plies were prepared and exposed to a plasma torch for 20 s with a heat flux of 16.5 MW/sq m at approximately 1650 C. Low erosion rates and little char formation were observed, confirming that these materials were promising for rocket motor nozzle materials. When fiber loadings increased, mechanical properties and ablative properties improved. The VGCF composites had low thermal conductivities (approximately 0.56 W/m-C) indicating they were good insulating materials. If a 65% fiber loading in VGCF composite can be achieved, then ablative properties are projected to be comparable to or better than the composite material currently used on the Space Shuttle Reusable Solid Rocket Motor (RSRM).

Patton, R. D.↗

Quantitation of Trace Water in ISS Atmosphere Samples Recovered from CO2-Removal Systems

As crewed spaceflight continues to push the limits of exploration, instruments and hardware used to maintain and monitor crew and vehicle health must become more integrated, reliable, and efficient. By combining a carbon dioxide (CO2) removal system with a resource recovery system like a Sabatier or Bosch reactor, the waste gas from the removal system can be converted into valuable resources that help reduce reliance on ground resupply. Due to the high-pressure nature of the Sabatier and Bosch reactions, the vent gas from most CO2 removal systems will need to be compressed before it can be processed. In order to prevent condensation in the compressor of the recovery system, it is critical to ensure that the vent stream from the CO2 removal system does not contain an excess of water. There are currently three different CO2 removal systems that are being developed as candidates for exploration missions. Each of these systems will be evaluated as a technology demonstration on ISS, and vent gas samples will be collected in Summa sampling canisters fitted with Entech valves. Due to the need to measure low levels of water in these samples, it was not possible to use the current ISS miniature grab sample containers (GSCs) to collect these samples. The Summa containers, which were used to collect archive samples during Shuttle missions, have a different surface treatment that makes it possible to measure the low levels of water in samples collected in these containers. This paper will provide some background on the CO2 removal systems being evaluated for exploration missions as well as results from ground-based testing of the current miniature GSCs and Summa canisters. Details on the development of the analytical method and the plan for preparing the canisters that will be used for in-flight sampling are also discussed.

Steven W Beck↗

Reporting Verification of BOP Shear Ram Capability: Requirements and Good Practices on Reporting Blowout Preventer (BOP) Shear Ram Capability for Outer Continental Shelf (OCS) Oil and Gas Operations

The Bureau of Safety and Environmental Enforcement (BSEE) Well Control Rule (Subpart G)1 became effective on July 28, 2016. This rule is part of the BSEE regulations pertaining to well control equipment used for oil and gas operations on the U.S. Outer Continental Shelf (OCS). More recently BSEE issue a proposed rule to amend portions of the 2016 well control rule. This proposed rule (now implemented) appeared in the Federal Register on May 18, 2018. This report was prepared late in the public comment period for the current rule and intended is a sample of desirable documentation of blind shear ram shear testing and associated regulatory requirements either in place or anticipated at the time of preparation. In accordance with this original rule and the proposed revisions, BSEE requests specific information regarding the capabilities of blind shear rams (BSR) in the Blowout Preventer (BOP). This information is required prior to beginning any operation involving the use of any BOP. More specifically, Title 30 CFR 250.732(b) of these regulations requires documentation of shear testing demonstrating the shearing and sealing capabilities of the BOP BSR. Such documentation is consistent with and complementary to other documentation verifying the designs of individual well control components and the overall BOP system. Verification demonstrates performance and reliability of the equipment based on a testing process that is repeatable and reproducible.2 This document, an annotated outline of verification documentation, arises from the combination of regulations and good practices concerning how to report BOP shear ram tests and third-party verification of BSR capability to support BSEE’s regulatory role.

03 NATURAL GAS↗