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At least 613 records · Page 34

'Bootstrap' Configuration for Multistage Pulse-Tube Coolers

A bootstrap configuration has been proposed for multistage pulse-tube coolers that, for instance, provide final-stage cooling to temperatures as low as 20 K. The bootstrap configuration supplants the conventional configuration, in which customarily the warm heat exchangers of all stages reject heat at ambient temperature. In the bootstrap configuration, the warm heat exchanger, the inertance tube, and the reservoir of each stage would be thermally anchored to the cold heat exchanger of the next warmer stage. The bootstrapped configuration is superior to the conventional setup, in some cases increasing the 20 K cooler's coefficient of performance two-fold over that of an otherwise equivalent conventional layout. The increased efficiency could translate into less power consumption, less cooler mass, and/or lower cost for a given amount of cooling.

Nguyen, Bich↗

Extending the low-temperature operation of sodium metal batteries combining linear and cyclic ether-based electrolyte solutions

Nonaqueous sodium-based batteries are ideal candidates for the next generation of electrochemical energy storage devices. However, despite the promising performance at ambient temperature, their low-temperature (e.g., < 0 °C) operation is detrimentally affected by the increase in the electrolyte resistance and solid electrolyte interphase (SEI) instability. Here, to circumvent these issues, we propose specific electrolyte formulations comprising linear and cyclic ether-based solvents and sodium trifluoromethanesulfonate salt that are thermally stable down to –150 °C and enable the formation of a stable SEI at low temperatures. When tested in the Na||Na coin cell configuration, the low-temperature electrolytes enable long-term cycling down to –80 °C. Via ex situ physicochemical (e.g., X-ray photoelectron spectroscopy, cryogenic transmission electron microscopy and atomic force microscopy) electrode measurements and density functional theory calculations, we investigate the mechanisms responsible for efficient low-temperature electrochemical performance. We also report the assembly and testing between –20 °C and –60 °C of full Na||Na 3 V 2 (PO 4 ) 3 coin cells. The cell tested at –40 °C shows an initial discharge capacity of 68 mAh g –1 with a capacity retention of approximately 94% after 100 cycles at 22 mA g –1 .

25 ENERGY STORAGE↗

Promoted Metals Combustion at Ambient and Elevated Temperatures

Promoted combustion testing of materials, Test 17 of NASA STD-6001, has been used to assess metal propensity to burn in oxygen rich environments. An igniter is used at the bottom end of a rod to promote ignition, and if combustion is sustained, the burning progresses from the bottom to the top of the rod. The physical mechanisms are very similar to the upward flammability test, Test 1 of NASA STD-6001. The differences are in the normal environmental range of pressures, oxygen content, and sample geometry. Upward flammability testing of organic materials can exhibit a significant transitional region between no burning to complete quasi-state burning. In this transitional region, the burn process exhibits a probabilistic nature. This transitional region has been identified for metals using the promoted combustion testing method at ambient initial temperatures. The work given here is focused on examining the transitional region and the quasi-steady burning region both at conventional ambient testing conditions and at elevated temperatures. A new heated promoted combustion facility and equipment at Marshall Space Flight Center have just been completed to provide the basic data regarding the metals operating temperature limits in contact with oxygen rich atmospheres at high pressures. Initial data have been obtained for Stainless Steel 304L, Stainless Steel 321, Haynes 214, and Inconel 718 at elevated temperatures in 100-percent oxygen atmospheres. These data along with an extended data set at ambient initial temperature test conditions are examined. The pressure boundaries of acceptable, non-burning usage is found to be lowered at elevated temperature.

Engel, Carl D.↗

Proton-bound cluster ions in ion mobility spectrometry

Gaseous oxygen and nitrogen bases, both singly and as binary mixtures, have been introduced into ion mobility spectrometers to study the appearance of protonated molecules, and proton-bound dimers and trimers. At ambient temperature it was possible to simultaneously observe, following the introduction of molecule A, comparable intensities of peaks ascribable to the reactant ion (H2O)nH+, the protonated molecule AH+ and AH+ H2O, and the symmetrical proton bound dimer A2H+. Mass spectral identification confirmed the identifications and also showed that the majority of the protonated molecules were hydrated and that the proton-bound dimers were hydrated to a much lesser extent. No significant peaks ascribable to proton-bound trimers were obtained no matter how high the sample concentration. Binary mixtures containing molecules A and B, in some cases gave not only the peaks unique to the individual compounds but also peaks due to asymmetrical proton bound dimers AHB+. Such ions were always present in the spectra of mixtures of oxygen bases but were not observed for several mixtures of oxygen and nitrogen bases. The dimers, which were not observable, notable for their low hydrogen bond strengths, must have decomposed in their passage from the ion source to the detector, i.e. in a time less than approximately 5 ms. When the temperature was lowered to -20 degrees C, trimers, both homogeneous and mixed, were observed with mixtures of alcohols. The importance of hydrogen bond energy, and hence operating temperature, in determining the degree of solvation of the ions that will be observed in an ion mobility spectrometer is stressed. The possibility is discussed that a displacement reaction involving ambient water plays a role in the dissociation.

Non-NASA Center↗

Microstructure of Methylammonium Lead iodide Perovskite Thin Films: A Comprehensive Study of the Strain and Texture

Controlling the microstructure of hybrid halide perovskite thin films is essential for optimizing their performance in optoelectronic devices. It is well established that the strain state of the perovskite layer affects its stability. Likewise, the orientation of the perovskite lattice is a determining parameter as these materials have shown pronounced anisotropies in their physical and mechanical properties. In this work, the authors focus on the understanding of the mechanisms that govern the strain and texture observed in MAPbI 3 thin films deposited on various oxide substrates. A thorough study of the evolution of the strain of the perovskite layer upon cooling down to room temperature from the crystallization temperature (100 °C) shows an essentially relaxed behavior of the perovskite layers. This result contradicts the commonly accepted hypothesis according to which MAPbI 3 layers synthesized above ambient temperature are strained due to the large mismatch in the thermal expansion coefficients of the perovskite and its substrate. The texture in MAPbI 3 layers is investigated by means of synchrotron full-field diffraction X-ray microscopy. This technique allows the direct observation of the [hh0] and [00l]-oriented domains at the origin of the observed textures, demonstrating both their twin and ferroelastic nature. The stability of the different domain orientations is investigated by DFT calculations, illustrating the determining role of the chemical environment at the film-substrate interface. PbI 2- terminated surfaces are found to favor the [hh0] orientations while for MAI-terminated ones, both [hh0] and [00l] domains are equally stabilized. The different results constitute an important step of clarification and understanding from the perspective of controlling the microstructure of perovskite layers.

36 MATERIALS SCIENCE↗

LUBRICATING PROPERTIES OF CERAMIC-BONDED CALCIUM FLUORIDE COATINGS ON NICKEL-BASE ALLOYS FROM 75 DEG TO 1900 DEG F

The endurance life and the friction coefficient of ceramic-bonded calcium fluoride (CaF2) coatings on nickel-base alloys were determined at temperatures from 75° to 1900° F. The specimen configuration consisted of a hemispherical rider (3/16-in. rad.) sliding against the flat surface of a rotating disk. Increasing the ambient temperature (up to 1500° F) or the sliding velocity generally reduced the friction coefficient and improved coating life. Base-metal selection was critical above 1500° F. For instance, cast Inconel sliding against coated Inconel X was lubricated effectively to 1500° F, but at 1600° F severe blistering of the coatings occurred. However, good lubrication and adherence were obtained for René 41 sliding against coated René 41 at temperatures up to 1900° F; no blisters developed, coating wear life was fairly good, and the rider wear rate was significantly lower than for the unlubricated metals . Friction coefficients were 0.12 at 1500° F, 0.15 at 1700° F, and 0.17 at 1800° and 1900° F. Because of its ready availability, Inconel X appears to be the preferred substrate alloy for applications in which the temperature does not exceed 1500° F. René 41 would have to be used in applications involving higher temperatures. Improved coating life was derived by either preoxidizing the substrate metals prior to the coating application or by applying a very thin (<0.0002 in.) burnished and sintered overlay to the surface of the coating. Preoxidation did not affect the friction coefficient. The overlay generally resulted i n a higher friction coefficient than that obtained without the overlay. The combination of both modifications resulted in longer coating life and in friction coefficients intermediate between those obtained with either modification alone.

Nickel alloy↗

Manufactured Porous Ambient Surface Simulants

The planetary science decadal survey for 2013-2022 (Vision and Voyages, NRC 2011) has promoted mission concepts for sample acquisition from small solar system bodies. Numerous comet-sampling tools are in development to meet this standard. Manufactured Porous Ambient Surface Simulants (MPASS) materials provide an opportunity to simulate variable features at ambient temperatures and pressures to appropriately test potential sample acquisition systems for comets, asteroids, and planetary surfaces. The original "flavor" of MPASS materials is known as Manufactured Porous Ambient Comet Simulants (MPACS), which was developed in parallel with the development of the Biblade Comet Sampling System (Backes et al., in review). The current suite of MPACS materials was developed through research of the physical and mechanical properties of comets from past comet missions results and modeling efforts, coordination with the science community at the Jet Propulsion Laboratory and testing of a wide range of materials and formulations. These simulants were required to represent the physical and mechanical properties of cometary nuclei, based on the current understanding of the science community. Working with cryogenic simulants can be tedious and costly; thus MPACS is a suite of ambient simulants that yields a brittle failure mode similar to that of cryogenic icy materials. Here we describe our suite of comet simulants known as MPACS that will be used to test and validate the Biblade Comet Sampling System (Backes et al., in review).

Carey, Elizabeth M.↗

Stable Thermotropic 3D and 2D Double Gyroid Nanostructures with Sub-2-nm Feature Size from Scalable Sugar–Polyolefin Conjugates

In this study, ultra-low molecular weight disaccharide–polyolefin conjugates with cellobiose, lactose and maltose head groups and atactic polypropene tails, such as 1, undergo a series of irreversible thermotropic order–order transitions with increasing temperature to provide nanostructured phases in the sequence: lamellar (L), hexagonal perforated lamellar (HPL), double gyroid (DG) and hexagonal cylindrical (C). The DG phase displays exceptional stability at ambient temperature and features two interpenetrating sugar domain networks having a sub-2-nm strut width and a lattice parameter, a DG , of 13.1 nm. The unique stability of this DG phase extends further within ultrathin films all the way down to the two-dimensional limit of 15 nm in which film thickness, l, is now less than the surface-oriented unit cell height, h DG . In addition to raising the fundamental question of what minimally constitutes a Schoen triply periodic minimal surface and DG lattice, these results serve to establish the class of sugar–polyolefin conjugates as a new material platform for nanoscience and nanotechnology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Stable Thermotropic 3D and 2D Double Gyroid Nanostructures with Sub‐2‐nm Feature Size from Scalable Sugar–Polyolefin Conjugates

Abstract Ultra‐low molecular weight disaccharide–polyolefin conjugates with cellobiose, lactose and maltose head groups and atactic polypropene tails, such as 1 , undergo a series of irreversible thermotropic order–order transitions with increasing temperature to provide nanostructured phases in the sequence: lamellar ( L ), hexagonal perforated lamellar ( HPL ), double gyroid ( DG ) and hexagonal cylindrical ( C ). The DG phase displays exceptional stability at ambient temperature and features two interpenetrating sugar domain networks having a sub‐2‐nm strut width and a lattice parameter, a DG , of 13.1 nm. The unique stability of this DG phase extends further within ultrathin films all the way down to the two‐dimensional limit of 15 nm in which film thickness, l , is now less than the surface‐oriented unit cell height, h DG . In addition to raising the fundamental question of what minimally constitutes a Schoen triply periodic minimal surface and DG lattice, these results serve to establish the class of sugar–polyolefin conjugates as a new material platform for nanoscience and nanotechnology.

Nowak, Samantha R.↗

Structural stability of mechanically alloyed amorphous (FeCoNi) 70 Ti 10 B 20 under high-temperature and high-pressure

Nanostructured (FeCoNi) 70 Ti 10 B 20 (at%) alloy was synthesized by mechanical alloying from elemental powder mixture of Fe, Co, Ni, Ti and B using ball milling. The effect of ball milling time on the evolution of structure and morphology was investigated by X-ray diffraction, scanning and transmission electron microscopy and differential thermal analysis. It was observed that the formation of solid solution of (FeCoNi) 70 Ti 10 B 20 started from the very onset of the milling process. Crystallite size and lattice strains seemed to be leveled off after 20 h of milling with no further major changes. The milling process for longer periods introduced severe plastic deformations causing formation of amorphous phase of (FeCoNi) 70 Ti 10 B 20 . The amorphous alloy composition was confirmed by energy dispersive X-ray spectroscopy analysis that showed an excellent homogeneity of the alloying elements. The phase stability of the mechanically alloyed amorphous sample was further verified by employing high-temperature and high-pressure studies. The alloy samples heat-treated at 700 °C revealed crystallization of the amorphous phase. However, synchrotron-based high-pressure ambient temperature X-ray diffraction studies confirmed that the amorphous phase of the alloy remained stable up to the pressure of 30 GPa. Here, the 50 h milled sample after being annealed at 350 °C showed improvement in the soft magnetic properties of the alloy, which was due to the probable elimination of the residual stress in the amorphous phase of the alloy powders.

36 MATERIALS SCIENCE↗

In situ observation of the deformation and fracture of an alumina-alumina ceramic-matrix composite at elevated temperature using x-ray computed tomography

The deformation and fracture of a 0/90° Nextel 720 mullite fibre / alumina matrix ceramic-matrix composite material has been observed by in situ synchrotron x-ray computed micro-tomography at ambient temperature and at 1100 °C. A three-point loading configuration was used and samples were loaded monotonically until final fracture. Here, the flexural strength was found to be unaffected by temperature. 3D visualisation of the microstructure showed fracture occurred by propagation of internal cracks at stresses close to the flexural strength. Shear fractures propagated across fibre bundles that were oriented perpendicular to the flexural stress at both room temperature and 1100 °C. At the higher temperature, an additional failure mode of delamination was observed, that may arise from relaxation of thermal residual stresses and creep.

36 MATERIALS SCIENCE↗

Adsorption of Iodine on Metal Coupons in Humid and Dry Environments

In this study, five different metal coupons were evaluated for gaseous iodine [I2(g)] adsorption including two stainless steels (i.e., SS304 and SS316), two Inconel® alloys (i.e., 625 and 718) and pure Ni (i.e., Ni-200) within a dynamic flow-through system where temperature, iodine concentration, flow rate, atmosphere, and relative humidity were controlled. Humidity was shown to be critical to iodine adsorption on SS304 and SS316 and Ni-200 at ambient temperatures. The results presented herein suggest that a moisture mediated reaction is occurring. However, higher humidity levels decrease the adsorption, suggesting an ideal range of humidity for highest corrosion. A comparison of the five metal substrates showed the highest I2(g) adsorption in the following descending order Ni-200 > SS304 > SS316 >718>625.The 625 and 718 Inconel alloys were fairly inert to iodine adsorption under the conditions tested. Characterization by scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction of the Ni-200 coupon indicates that NiI2 is formed and flakes off the surface as a black powder. The SS304 and SS316 coupons showed evidence of extensive reactions with I2(g) and formed a much more deliquescent corrosion product, which reacted with air when removed from the flow-through system for weighing on the analytical balance. These findings assist in predicting iodine adsorption behavior on a variety of metal surfaces under various conditions.

Beck, Chelsie L.↗

Coaxial laser absorption and optical emission spectroscopy of high-pressure aluminum monoxide

This work advances laser absorption spectroscopy with measurements of aluminum monoxide (AlO) temperature and column density in extreme pressure ( P > 60 bar) and temperature ( T > 4000 K) environments. Measurements of the AlO A 2 Π i – X 2 Σ + transition are made using a microelectromechanical system, tunable vertical cavity surface emitting laser (MEMS-VCSEL). Simultaneous emission measurements of the AlO B 2 Σ + – X 2 Σ + transition are made along a line of sight that is coaxial with the laser absorption. Absorption temperature fits agree with emission spectra for a T = 3200 K, P = 9 bar case. In cases with T > 4000 K, P > 60 bar, absorption fits match the ambient temperature while emission fits over-estimate it, owing to high optical depths. These data juxtapose passive and active spectroscopic methods and demonstrate the versatility of AlO laser absorption in high-pressure and high-temperature environments where experimental data remain scarce, and engineering models will benefit from refined measurements.

Daniel, K. A.↗

Creep rupture behavior of unidirectional advanced composites

A 'material modeling' methodology for predicting the creep rupture behavior of unidirectional advanced composites is proposed. In this approach the parameters (obtained from short-term tests) required to make the predictions are the three principal creep compliance master curves and their corresponding quasi-static strengths tested at room temperature (22 C). Using these parameters in conjunction with a failure criterion, creep rupture envelopes can be generated for any combination of in-plane loading conditions and ambient temperature. The analysis was validated experimentally for one composite system, the T300/934 graphite-epoxy system. This was done by performing short-term creep tests (to generate the principal creep compliance master curves with the time-temperature superposition principle) and relatively long-term creep rupture tensile tests of off-axis specimens at 180 C. Good to reasonable agreement between experimental and analytical results is observed.

Yeow, Y. T.↗

Lubricating Properties of Ceramic-Bonded Calcium Fluoride Coatings on Nickel-Base Alloys from 75 to 1900 deg F

The endurance life and the friction coefficient of ceramic-bonded calcium fluoride (CaF2) coatings on nickel-base alloys were determined at temperatures from 75 F to 1900 F. The specimen configuration consisted of a hemispherical rider (3/16-in. rad.) sliding against the flat surface of a rotating disk. Increasing the ambient temperature (up to 1500 F) or the sliding velocity generally reduced the friction coefficient and improved coating life. Base-metal selection was critical above 1500 F. For instance, cast Inconel sliding against coated Inconel X was lubricated effectively to 1500 F, but at 1600 F severe blistering of the coatings occurred. However, good lubrication and adherence were obtained for Rene 41 sliding against coated Rene 41 at temperatures up to 1900 F; no blisters developed, coating wear life was fairly good, and the rider wear rate was significantly lower than for the unlubricated metals. Friction coefficients were 0.12 at 1500 F, 0.15 at 1700 F, and 0.17 at 1800 F and 1900 F. Because of its ready availability, Inconel X appears to be the preferred substrate alloy for applications in which the temperature does not exceed 1500 F. Rene 41 would have to be used in applications involving higher temperatures. Improved coating life was derived by either preoxidizing the substrate metals prior to the coating application or by applying a very thin (less than 0.0002 in.) burnished and sintered overlay to the surface of the coating. Preoxidation did not affect the friction coefficient. The overlay generally resulted in a higher friction coefficient than that obtained without the overlay. The combination of both modifications resulted in longer coating life and in friction coefficients intermediate between those obtained with either modification alone.

Sliney, Harold E.↗