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At least 91 records · Page 5

Demonstration of rapid and sensitive module leak certification for Space Station Freedom

A leak detection and quantification demonstration using perflurocarbon tracer (PFT) technology was successfully performed at the NASA Marshall Space Flight Center on January 25, 1991. The real-time Dual Trap Analyzer (DTA) at one-half hour after the start of the first run gave an estimated leak rate of 0.7 mL/min. This has since been refined to be 1.15 (+ or -) 0.09 mL/min. The leak rates in the next three runs were determined to be 9.8 (+ or -) 0.7, -0.4 (+ or -) 0.3, and 76 (+ or -) 6 mL/min, respectively. The theory on leak quantification in the steady-state and time-dependent modes for a single zone test facility was developed and applied to the above determinations. The laboratory PFT analysis system gave a limit-of-detection (LOD) of 0.05 fL for ocPDCH. This is the tracer of choice and is about 100-fold better than that for the DTA. Applied to leak certification, the LOD is about 0.00002 mL/s (0.000075 L/h), a 5 order-of-magnitude improvement over the original leak certification specification. Furthermore, this limit can be attained in a measurement period of 3 to 4 hours instead of days, weeks, or months. A new Leak Certification Facility is also proposed to provide for zonal (three zones) determination of leak rates. The appropriate multizone equations, their solutions, and error analysis have already been derived. A new concept of seal-integrity certification has been demonstrated for a variety of controlled leaks in the range of module leak testing. High structural integrity leaks were shown to have a linear dependence of flow on (Delta)p. The rapid determination of leak rates at different pressures is proposed and is to be determined while subjecting the module to other external force-generating parameters such as vibration, torque, solar intensity, etc.

Dietz, R. N.↗

A DTA/GC for the in Situ Identification of the Martian Surface Material

The composition and mineralogy of the Martian surface material remain largely unknown. To determine its composition and mineralogy, several techniques are being considered for in situ analyses of the Martian surface material during missions to Mars. We have successfully developed, constructed, and tested a laboratory DTA/GC. The DTA is a Dupont model 1600 high temperature DTA coupled with a GC equipped with a MID detector. The system is operated by a Sun Sparc 11 workstation. When gas evolves during a thermal chemical event, it is shunted into the GC and the temperature is recorded in association with the specific thermal event. We have used this laboratory instrument to define experimental criteria necessary for determining the composition and mineralogy of the Martian surface in situ (e.g., heating of sample to 1100 C to distinguish clays). Our studies indicate that DTA/GC will provide a broad spectrum of mineralogical and evolved gas data pertinent to exobiology, geochemistry, and geology.

Mancinelli, R. L.↗

Magnetite: What it reveals about the origin of the banded iron formations

Magnetite, Fe3O4 is produced abiotically and biotically. Abiotically, magnetite is a late magmatic mineral and forms as a consequence of the cooling of iron rich magma. Biotically, magnetite is produced by several organisms, including magnetotactic bacteria. Hematite, Fe2O3, is also produced abiotically and biotically. Abiotically, hematite rarely occurs as a primary mineral in igneous rocks, but is common as an alteration product, fumarole deposit, and in some metamorphosed Fe-rich rocks. Biotically, hematite is produced by several types of microorganisms. Biologically-produced magnetite and hematite are formed under the control of the host organism, and consequently, have characteristics not found in abiotically produced magnetite and hematite crystals. To determine if the magnetite and hematite in the Banded Iron Formation was biologically or abiotically produced, the characteristics of biologically-produced magnetite and hematite (concentrated from Aquaspirillum magnetotacticum) and abiotically-produced magnetite and hematite obtained from Wards Scientific Supply Company, were compared with characteristics of magnetite and hematite concentrated from the Gunflint Banded Iron Formation (Ontario, Canada) using thermal and crystallographic analytical techniques. Whole rock analysis of the Gunflint Banded Iron Formation by x-ray diffraction (XRD) and differential thermal analysis (DTA) revealed the presence of quartz, hematite, siderite and dolomite as the major minerals, and magnetite, greenalite, pyrite, pyrrhotite and apatite as the minor minerals. Analysis of a crude magnetic fraction of the Gunflint showed the minerals quartz, hematite, siderite, dolomite, and magnetite. Analysis of the crude magnetic fraction from Aquaspirillum magnetotacticum revealed organic compounds plus hematite and magnetite. The mineral identification and particle size distribution data obtained from the DTA along with XRD data indicate that the magnetite and hematite from the Gunflint BIF share some similarities with biologically formed magnetite and hematite.

Schwartz, D. E.↗

The role of silver in the processing and properties of Bi-2212

The influence of the silver content and the oxygen partial pressure on the solidus temperature and the weight loss during melting of Bi2Sr2Ca1Cu2O(x) has been examined by means of DTA and TGA. By decreasing the oxygen partial pressure the solidus is lowered (e.g. del T = 59 C by decreasing pO2 from 1 atm to 0.001 atm) and the weight loss is increased. The addition of silver causes two effects: (1) the solidus is further decreased (e.g. 2 wt% Ag lower T (solidus) by up to 25 C, depending on the oxygen partial pressure); and (2) the weight loss during melting is reduced. Thick films (10-20 micron in thickness) with 0 and 5 wt% silver and bulk samples with) and 2.7 wt% silver were melt processed in flowing oxygen on a silver substrate in the DTA, allowing the observation of the melting process and a good temperature control. The critical current densities are vigorously dependent on the maximum processing temperature. The highest j(sub c) in thick films (8000 A/sq cm at 77 K, O T) was reached by melting 7 C above the solidus temperature. The silver addition shows no significant effect on the processing parameters or the superconducting properties. The highest j(sub c) for bulk samples (1 mm in thickness) was obtained by partial melting at 900 C or 880 C, depending on the silver content of the powder (0 or 2.7 wt%). The j(sub c) of the samples is slightly enhanced from 1800 A/sq cm (at 77 K, O T) to 2000 A/sq cm by the silver addition. To be able to reach at least 80% of the maximum critical current density, the temperature has to be controlled in a window of 5 C for thick films and 17 C for bulk samples.

Lang, TH.↗

A Preliminary Investigation of the Cr3Si-Mo Pseudo-Binary Phase Diagram

An investigation was undertaken to study the phase relations in Cr3Si alloyed with Mo varying from 10 to 83.5 wt. % of the material. Specimens were prepared from arc-melted buttons that were subsequently heat treated at 1673 K for 200 h and air quenched to room temperature to structures. Alloys containing more than 20 wt. % MO were primarily two-phase materials of M3Si and M5Si3, where M is (Cr,Mo). Three alloys contained less than 5% of a third phase, which also had the M5Si3 crystal structure. Differential thermal analysis (DTA) was performed on several specimens at temperatures up to 2073 K in order to determine a solidus curve for the M3Si phase. Since only one DTA peak was observed in each alloy, the M5Si3 phase must melt above 2073 K, the maximum temperature examined. A preliminary pseudo-binary phase diagram for (Cr,Mo)3Si and a portion of the 1673 K isothermal section of the Cr-Mo-Si ternary phase diagram are presented.

Dickerson, R. M.↗

Non-Isothermal Calorimetric Studies of the Crystallization of Lithium Disilicate Glass

The influence of preannealing treatments on the polymorphic crystallization of lithium disilicate glasses is examined. As expected, glasses heated at different rates through the temperature range where there is significant nucleation develop widely different numbers of nuclei. This can dramatically influence the stability and transformation characteristics of the annealed glass. Non-isothermal differential scanning calorimetry (DSC) and differential thermal analysis (DTA) measurements are demonstrated to be useful to probe the nucleation behavior. The first systematic investigations of particle size effects on the non-isothermal transformation behavior are presented and discussed. Based on DTA and microscopy experiments, we show that small particles of lithium disilicate glasses crystallize primarily by surface crystallization. The relative importance of surface versus volume crystallization is examined by varying particle size, by introducing nucleating agents and by exposing glasses to atmospheres of different water content. These data are analyzed quantitatively using a numerical model developed in a second paper following in this volume.

Ray, C. S.↗

Differential Thermal Analysis of Hg(1-x)Mn(x)Te Alloys in the X=0 to 0.3 Range

Understanding the experimental conditions necessary for the development of radial and axial compositional homogeneity in directionally solidified Hg(0.89)Mn(0.11)Te(MMT) crystals has been difficult due to the lack of segregation coefficient data on the Hg(1-x)Mn(x)Te alloy system in the X = 0 to 0.3 composition range. Determining segregation coefficient data from the available Hg(1-x)Mn(x)Te alloy phase equilibria data is not practical due to discrepancies in the shape of the reported solidus and liquidus curves in the X = 0 to 0.3 range. To resolve these discrepancies and to obtain segregation coefficient data which can be used to understand homogeneity in directionally solidified MMT crystals, the solidus and liquidus temperatures of seven Hg(1-x)Mn(x)Te alloys in the X = 0 to 0.3 range were determined using differential thermal analysis (DTA). The Hg(1-x)Mn(x)Te phase diagram constructed for the X = 0 to 0.3 range of this alloy system from the DTA measurements clarifies the shape of the solidus and liquidus curves in this range. The segregation coefficient for the Hg(1-x)Mn(x)Te system was found to vary from 5 to 4.4 as the solidus composition increased from 0-30 atomic percent MnTe. This information will be useful in the analysis of axial and radial homogeneity of directionally solidified MMT crystals.

Price, M. W.↗

Crystallization Kinetics of a Solid Oxide Fuel Cell Seal Glass by Differential Thermal Analysis

Crystallization kinetics of a barium calcium aluminosilicate glass (BCAS), a sealant material for planar solid oxide fuel cells, have been investigated by differential thermal analysis (DTA). From variation of DTA peak maximum temperature with heating rate, the activation energy for glass crystallization was calculated to be 259 kJ/mol. Development of crystalline phases on thermal treatments of the glass at various temperatures has been followed by powder x-ray diffraction. Microstructure and chemical composition of the crystalline phases were investigated by scanning electron microscopy and energy dispersive spectroscopic (EDS) analysis. BaSiO3 and hexacelsian (BaAl2Si2O8) were the primary crystalline phases whereas monoclinic celsian (BaAl2Si2O8) and (Ba(x), Ca(y))SiO4 were also detected as minor phases. Needle-shaped BaSiO3 crystals are formed first, followed by the formation of other phases at longer times of heat treatments. The glass does not fully crystallize even after long term heat treatments at 750 to 900 C.

Bansal, Narottam P.↗

Mars Geochemical Instrument (MarGI): An instrument for the analysis of the Martian surface and the search for evidence of life

The Mars Geochemical Instrument, MarGI, was developed to provide a comprehensive analysis of the rocks and surface material on Mars. The instrument combines Differential Thermal Analysis (DTA) with miniature Gas Chromatography-Ion Mobility Spectrometry (GC-IMS) to identify minerals, the presence and state of water, and organic compounds. Miniature pyrolysis ovens are used to both, conduct DTA analysis of soil or crushed rocks samples, and pyrolyze the samples at temperatures up to 1000 degrees C for GC-IMS analysis of the released gases. This combination of analytical processes and techniques, which can characterize the mineralogy of the rocks and soil, and identify and quantify volatiles released during pyrolysis, has applications across a wide range of target sites including comets, planets, asteroids, and moons such as Titan and Europa. The MarGI analytical approach evolved from the Cometary Ice and Dust Experiment (CIDEX) selected to fly on the Comet Rendezvous Asteroid Flyby Mission (CRAF).

Kojiro, Daniel R.↗

Gas-Granular Simulation Framework for Spacecraft Landing Plume-Surface Interaction and Debris Transport Analysis

The Gas-Granular Flow Solver (GGFS) multi-phase flow computational framework has been developed to enable simulations of particle flows complex extra-terrestrial regolith materials. Particle flows of interest include the damage of unprepared landing sites from rocket plume impingement on Moon, Mars, and asteroids. The flow solver implements an Eulerian-Eulerian two-fluid model with fluid representation of the gas phase and granular phase to avoid the need to model billions of particle interactions. The granular phase is modeled as an Eulerian fluid with constituent physics closure models derived from first-principle Discrete Element Model (DEM) particle interaction simulations that capture the complex, non-linear granular particle interaction effects. Granular phase constituent models have been developed and integrated that address the complex, non-linear granular material mechanics complexities resulting from both: the irregular, jagged particle shapes and poly-disperse mixture effects encountered in extra-terrestrial regolith, with lunar regolith as the extreme. The GGFS capabilities are being integrated into a proven NASA plume-surface interaction and debris transport simulation framework featuring the Loci/CHEM CFD program and Debris Transport Analysis (DTA) post-processing tools for applications in robotic and human Moon and Mars lander development. Integration of the three simulation tool components. Loci/CHEM, GGFS, and DTA, into a coordinated simulation framework will enable time-accurate spacecraft landing simulations that account for the alteration of the landing surface through plume-induced cratering and the resulting redirection of plume impingement flow and debris transport. Initial implementation of this simulation framework and application examples will be presented.

Liever, Peter A.↗

INL_Intern_Poster_ColeBailey [Poster]

Understanding the thermophysical properties of molten salts is crucial for the advancement of nuclear fuels. This project presents the design of a custom differential thermal analyzer (DTA) that utilizes non-contact ultrasonic mixing to agitate samples and prevent supercooling. The supercooling effect occurs when a liquid is below its freezing point without solidifying. This can be observed when a liquid in a freezer instantly transitions to its solid phase upon disturbance. By avoiding this effect, accurate transition temperatures of molten salts can be gathered for future applications. Initial mixing results were promising, leading to further refinement of the waveguides using ABAQUS to maximize input energy into the fluid. Future work will focus on integrating both mixing and cooling in conjunctions to observe the avoided effect.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

Hydrogen Induced Abrupt Structural Expansion at High Temperatures of a Ni 32 Nb 28 Zr 30 Cu 10 Membrane for H 2 Purification

Ni-Nb-Zr amorphous membranes, prepared by melt-spinning, show great potential for replacing crystalline Pd-based materials in the field of hydrogen purification to an ultrapure grade (>99.999%). In this study, we investigate the temperature evolution of the structure of an amorphous ribbon with the composition Ni 32 Nb 28 Zr 30 Cu 10 (expressed in atom %) by means of XRD and DTA measurements. An abrupt structural expansion is induced between 240 and 300 °C by hydrogenation. This structural modification deeply modifies the hydrogen sorption properties of the membrane, which indeed shows a strong reduction of the hydrogen capacity above 270 °C.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Crystallization Kinetics of Calcium-magnesium Aluminosilicate (CMAS) Glass

The crystallization kinetics of a calcium-magnesium aluminosilicate (CMAS) glass with composition relevant for aerospace applications, like air-breathing engines, were evaluated using differential thermal analysis (DTA) in powder and bulk forms. Activation energy and frequency factor values for crystallization of the glass were evaluated. X-ray diffraction (XRD) was used to investigate the onset of crystallization and the phases that developed after heat treating bulk glass at temperatures ranging from 690 to 960 deg for various times. Samples annealed at temperatures below 900 deg remained amorphous, while specimens heat treated at and above 900 deg exhibited crystallinity originating at the surface. The crystalline phases were identified as wollastonite (CaSiO3) and aluminum diopside (Ca(Mg,Al) (Si,Al)2O6). Scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS) were employed to examine the microstructure and chemical compositions of crystalline phases formed after heat treatment.

X-ray diffraction (XRD)↗

Synthesis, Spectral Characterization, Thermal and Optical Studies of Novel Complexes: 4-(Dimethylamino)benzylidene-4-acetamideaniline and 4-(Dimethylamino)benzylidene-4-nitroaniline

The phase diagram representing solid–liquid equilibrium of entire range of composition and thermodynamic studies of two binary organic systems of 4-dimethylaminobenzaldehyde (DMAB) with two NLO active compounds, p-aminoacetanilide (PAA) and p-nitroaniline (PNA), have been studied by solid state synthetic route. Both systems are independently forming a new entity called intermolecular complex (IMC) and two eutectics on either side of intermolecular complexes. The various thermodynamic parameters such as heat of mixing, entropy of fusion, roughness parameter, interfacial energy and excess thermodynamic functions of IMCs and eutectics were calculated using the heat of fusion values. The TGA and DTA studies were performed to understand the physico-chemical, thermal behavior and unique identity of newly synthesized organic complexes, 4-(dimethylamino)benzylidene-4-acetamideaniline (DMABPAA) and 4-(dimethylamino)benzylidene-4-nitroaniline (DMABPNA), and their respective enthalpy of fusion values were found to be 30.01 and 37.26 kJ mol{sup − 1}. The higher melting point of both the novel complexes than their parent’s compounds reveal the strong molecular interaction between parent components to yield the complex. The FTIR spectral analysis predicts the disappearance of aldehyde peaks of DMAB and NH{sub 2} peaks of PAA and PNA while the appearance of entirely new peaks than that of parent’s compounds are the supportive for the formation of new molecular entities. These findings are further supported by FTNMR spectrum studies by observation of disappearance of proton peak of aldehyde of DMAB and amine peaks of PAA and PNA rather formation of new imine proton peak or peaks were observed. The appearance of new peaks in Powder XRD of complexes than those of parent components is further indicative for the formation of complexes. The absorption spectrum of DMABPAA and DMABPNA showed intra-molecular charge-transfer (ICT) excited state absorption at 258 and 241 nm, respectively. Both the IMCs, DMABPAA and DMABPNA, show strong fluorescence with quantum yield 0.66 and 0.93, respectively, in methanol solution.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Spectro Analytical, Computational and In Vitro Biological Studies of Novel Substituted Quinolone Hydrazone and it’s Metal Complexes

Some novel transition metal [Cu (II), Ni (II) and Co (II)] complexes of nalidixic acid hydrazone have been prepared and characterized by employing spectro-analytical techniques viz: elemental analysis, {sup 1}H-NMR, Mass, UV–Vis, IR, TGA-DTA, SEM-EDX, ESR and Spectrophotometry studies. The HyperChem 7.5 software was used for geometry optimization of title compound in its molecular and ionic forms. Quantum mechanical parameters, contour maps of highest occupied molecular orbitals (HOMO) and lowest unoccupied molecular orbitals (LUMO) and corresponding binding energy values were computed using semi empirical single point PM3 method. The stoichiometric equilibrium studies of metal complexes carried out spectrophotometrically using Job’s continuous variation and mole ratio methods inferred formation of 1:2 (ML{sub 2}) metal complexes in respective systems. The title compound and its metal complexes screened for antibacterial and antifungal properties, exemplified improved activity in metal complexes. The studies of nuclease activity for the cleavage of CT- DNA and MTT assay for in vitro cytotoxic properties involving metal complexes exhibited high activity. In addition, the DNA binding properties of Cu (II), Ni (II) and Co (II) complexes investigated by electronic absorption and fluorescence measurements revealed their good binding ability and commended agreement of K{sub b} values obtained from both the techniques. Molecular docking studies were also performed to find the binding affinity of synthesized compounds with DNA (PDB ID: 1N37) and “Thymidine phosphorylase from E.coli” (PDB ID: 4EAF) protein targets.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Cobalt Oxide Nanoparticles on the Nano-scale Free Volume and Optical Properties of Biodegradable CMC/PVA Films

Chemically prepared cobalt oxide nanoparticles (NPs) were added to biodegradable carboxymethyl cellulose (CMC) (20%)/polyvinyl alcohol (PVA) (80%) blend films. The structural properties of these films were investigated by X-ray diffraction, Fourier transformation infrared spectroscopy (FTIR) and differential thermal analysis (DTA). Co{sub 3}O{sub 4}/(CMC + PVA) films show a semi-crystalline structure and the degree of crystallinity decreases with adding Co{sub 3}O{sub 4} NPs. FTIR confirms the good interaction between the blend chains and Co{sub 3}O{sub 4} NPs. The melting temperature T{sub m} for CMC/PVA is about 212 °C then decreased with increasing Co{sub 3}O{sub 4} content, due to some decrease in the ordered association of the blend which results in a decrease in the blend crystallinity. Positron annihilation lifetime spectroscopy (PALS) measurements were carried out with a conventional fast–fast coincidence spectrometer. It was found that ortho-positronium lifetime τ{sub 3} and free volume V{sub f} increase while o-Ps intensity I{sub 3} still constant as Co{sub 3}O{sub 4} concentration increases. This is because adding Co{sub 3}O{sub 4} NPs encourages the formation of o-Ps. The swelling ratio SR% as a function of Co{sub 3}O{sub 4} concentration was also studied and its value increases with Co{sub 3}O{sub 4} addition. The optical study illustrated the decrease of the transmittance T of the films from 87 to 35.5% with increasing Co{sub 3}O{sub 4} content from 0 to 0.9 wt%. Also, both the direct and indirect optical band gaps of the films red-shifted from 4.05 to 3.75 eV and 3.3 to 2.75 eV, respectively. The influence of Co{sub 3}O{sub 4} on the refractive index of the films is also reported.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Microwave-Hydrothermal Synthesis of Y{sub 3}Fe{sub 5}O{sub 12} Nanoparticles: Sintering Temperature Effect on Structural, Magnetic and Dielectric Properties

Herein, we report a facile microwave-assisted hydrothermal method for the preparation of yttrium iron garnet (YIG, Y{sub 3}Fe{sub 5}O{sub 12})nanocrystals and realized the synergy between its structural and magnetic properties. The as-prepared powder thermal stability was characterized in detail by using thermogravimetric-differential thermal analysis (TG-DTA). The synthesized powder was microwave sintered at six different temperatures ranging from 973 to 1373 K for 60 min and characterized using X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). Magnetic properties were investigated by vibrating-sample magnetometer (VSM) and ferromagnetic resonance (FMR) studies. The frequency variation of dielectric and magnetic properties was measured in the frequency range of 100 kHz–1.8 GHz. The observed magnetic and dielectric parameters such as saturation magnetization, coercivity, permeability, linewidth, dielectric constant and magnetodielectric losses are strongly affected by sintering temperature. The saturation magnetization and coercivity of YIG were found in the range 14.4–28.0 emu/g and 35–87 Oe, respectively. Furthermore, the FMR linewidth decreases from 844 to 204 Oe. This analysis undoubtedly demonstrates that the synthesis method and sintering temperature have the prominent effect on the electrical and magnetic properties of YIG and would be very useful for the garnet-based microwave device applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Spectral, Electrical, Thermoelectrical and Dielectric Properties of (Zn,Zr) Co-doped CuFe{sub 2}O{sub 4}

The effects of Zr{sup + 4} and Zn{sup + 2} substitution on the electrical, dielectric and spectral properties of non-stoichiometric Cu{sub 1−x}Zn{sub x}Zr{sub y}Fe{sub 2−y}O{sub 4+} {sub δ} and stoichiometric Cu{sub 1−x}Zn{sub x+} {sub y}Zr{sub y}Fe{sub 2−2y}O{sub 4} ferrites prepared by double sintering ceramic technique have been investigated. IR absorption spectra confirm the formion of spinel structure. On the other hand, IR spectra can give an idea about the change of molecular structure of ferrites system due to the perturbation that occurred in Fe{sup 3+}–O{sup 2−} bond by introducing Zn and Zr elements. The phase identification of nonstoichiometric (ns) and stoichiometric (s) samples was confirmed by the presence of endothermic peak from DTA curves at around 936 {sup ∘}C in agreement with X-ray diffraction and IR results. The calculated low values of activation energies for conduction are in the range that suggests the conduction is due to thermally activated mobility and the presence of hopping conduction mechanism. Thermoelectric power exhibits positive sign for most s and ns samples. The concentration of charge carrier is constant in the ferromagnetic region. It is also noted that the dielectric constant decreases with increasing Zn and Zr contents. From the above discussion the samples containing Zn and Zr elements have lower ΔB{sub pp} values with low energy loss. From the ESR analysis it can be confirmed that the addition of Zn and Zr generally decrease the power loss which is very important in the application for the manufacturing of a material which is used as a core of transformer at the microwave frequencies.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗