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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2017

Thermal Degradation Investigation of Polyurethane Elastomers using Thermal Gravimetric Analysis - Gas Chromatography/Mass Spectrometry

The thermal degradation of two polyurethane elastomers was investigated via thermal gravimetric analysis coupled with gas chromatography/ma ss spectrometry. Decomposition occur s in a multi - step fashion with similar onset temperatures for both materials. Apparent activation energy plots were calculated inside Model - Free Kinetics software and utilized to construct conversion and isothermal conversion tables . These tables predicted material degradation as a function of temperature and time. Isothermal experiments were performed and found to be in good agreement with the predictions made from the Model - Free Kinetic s software package. Volatile products evolved during the multistep decomposition were captured at various times and analyzed using the coupled gas chromatography/mass spectrometry system . This analysis demonstrated strong correlation between the degradation products and known decomposition mechanisms for polyurethanes.

36 MATERIALS SCIENCE↗
DOE OSTI2012

Effect of homolog doping on surface morphology and mass-loss rates from PETN crystals. Studies using atomic force microscope and thermo-gravimetric analysis

Pentaerythritol tetranitrate (PETN) is an important energetic material and its performance as a secondary explosive depends strongly on the density as well as flow porosity of powdered material, which in turn is governed by the size and surface properties of the PETN crystallite particles. Historically there has been evidence that the surface properties of PETN particles can be strongly influenced by the presence of homolog impurities of PETN, in particular, dipentaerythritol hexanitrate (diPEHN) and tripentaerythritol octanitrate (triPEON), although not many systematic studies characterizing such influence exist. In this work we employ thermogravimetric analysis (TGA) to measure mass-loss rates at elevated temperatures and show that doping with a small amount of diPEHN and triPEON can reduce the mass-loss rate from PETN single-crystal surfaces by as much as 35 % as compared to undoped crystals. Arrhenius plots of mass-loss rates as a function of temperature suggest that the reduction in evaporation is not due to the change in activation barrier of the molecular evaporation process, but perhaps due to the impedance to the receding motion of the steps by the immobile impurities on the surface. Removal of surface impurities through gentle washing with ethanol leads to enhanced mass-loss rate relative to pure PETN suggesting a roughened surface morphology. Some surface roughening in doped crystals is supported by Atomic force microscopy (AFM) images of growth layers that show evidences of growth layer stacking and rough edges. Furthermore, we find that a larger amount of impurity added to the original solution does not necessarily lead to a more highly doped crystal, which could perhaps be interpreted as PETN crystals being able to accommodate only up to a certain weight percent of homolog impurities.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1995

Replacement of ozone depleting and toxic chemicals in gravimetric analysis of non-volatile residue

The standard tests for determining nonvolatile residue accretion on spacecraft surfaces and in clean processing facilities rely on the use of halogenated solvents that are targeted for elimination because of their toxic or ozone-depleting natures. This paper presents a literature-based screening survey for candidate replacement solvents. Potential replacements were evaluated for their vapor pressure, toxicity, and solvent properties. Three likely candidates were identified: ethyl acetate, methyl acetate, and acetone. Laboratory tests are presented that evaluate the suitability of these candidate replacement solvents.

Arnold, G. S.↗
NASA NTRS2004

QCM Thermo-Gravimetric Analysis (QTGA) Comparisons

The ASTM E-1559 apparatus has been used for years at NASA/Goddard Space Flight Center (GSFC) to determine in situ outgassing rate information, as well as pertinent in situ TML and multiple VCM values. The apparatus also affords the opportunity to experimentally compute the evaporation rates of molecular species that are reemitted as the Quartz Crystal Microbalances (QCMs) are gradually warmed up at some controlled temperature. Typically the molecular mass that accumulates onto the test QCMs are a compilation of species that are outgassing from the sample due to their respective activation energies and the desorption processes that the sample undergoes at various tested temperatures. It has been speculated that if there is too much molecular buildup of condensed water vapor (ice) onto the QCM crystal that a significantly higher temperature would be needed to break these "ice" bonds. ASTM E-1559 data plots will be used to demonstrate the thermogravimetric effects of water and other miscible molecular species with various water/ice thicknesses and at different evaporation rates.

Rosecrans, Glenn↗
DOE OSTI2013

Tropical sea snail shells: Possible exotic sources for ceramic biomaterial synthesis

In this study, chemical and structural properties of sea snail shell based bioceramic materials (i.e. hydroxyapatite, whitlockite and other phases) are produced by using mechano-chemical (ultrasonic) conversion method. For this purpose, differential thermal and gravimetric analysis (DTA/TG), X-ray diffraction, infra-red (IR) and scanning electron microscope (SEM) studies are performed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

IWTU TI-102 – Part 2 Sample Analyses

Samples from the Integrated Waste Treatment Unit (IWTU) were collected for analysis after TI-102 – Part 2 shutdown. The scope of analyses performed by Battelle Energy Alliance (BEA) included: • Scanning electron micrography (SEM) and energy dispersive spectroscopy (EDS) analysis for particle morphology, particle size, and elemental composition estimates • Loss on ignition (LOI) for determining the fraction that is coke and not bauxite • Proximate and ultimate analysis • Particle-size analysis using sieve trays • Bulk and particle density • Elemental analysis • Solubility • X-ray diffraction for mineralogy analysis • Thermal gravimetric analysis (TGA). This report provides the results of those analyses.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1980

Incorporation of metal ions into polyimides

The effects of the incorporation of metal ions into various polyimides on polyimide properties are investigated. Polyimide films derived from 3,3',4,4'-benzophenone tetracarboxylic acid dianhydride (BDTA) 3,3'-diaminobenzophenone (m,m'-DABP), 4,4'-diaminobenzophenone (p,p'-DABP) or 4,4'-oxydianiline were prepared with the concurrent addition of approximately 20 metals in a variety of forms. In general, it is found that the films derived from BDTA + p,p'-DABP were brittle and of poor quality, with brittle films also produced in most of the BDTA + m, m'-DABP polyimides regardless of whether the added metal was hydrate or anhydrous. Thermomechanical analysis, torsional braid analysis, thermal gravimetric analysis, infrared spectral analysis and isothermal studies on many of the polyimide films produced indicate that the softening temperature is generally increased upon the addition of metal ions, at the expense of thermal stability, while no changes in chemical functionality are observed. The best system studied in regard to polymer property enhancement appears to be tri(acetylacetonato)aluminum(III) added to the m, m'-DABP polyamide, which has been found to exhibit four times the lap shear strength of the polyimide alone.

Taylor, L. T.↗
DOE OSTI2015

Investigation of intrinsic and extrinsic defects effective role on producing intense red emission in ZnO:Eu nanostructures

Highlights: • Effective role of defects on producing red emission at indirect excitation. • V{sub Zn} and V{sub O} defects have important role on energy transfer. • Mg related defects and Zn{sub i} defects were responsible for blue emission. • Extrinsic and intrinsic defects mediated energy transfer to sensitize Eu{sup 3+} ions. • Decrease of red emission because of diminishing in oxygen vacancy. - Abstract: Europium doped ZnO nanorads and nanosheets were synthesized by hydrothermal method. Effects of Mg doping, morphology and annealing in oxygen ambient on structural and optical properties of ZnO nanostructures were investigated using X-ray diffraction (XRD), particle size analysis (PSA), thermo gravimetric analysis (TGA), differential thermal analysis (DTA), differential thermo gravimetry (DTG), scanning electron microscopy (SEM) and photoluminescence spectroscopy (PL). This study recommends that both of intrinsic and extrinsic defects facilitate energy transfer (ET) from the ZnO host to Eu{sup 3+} ions and consequently have efficient role on producing intense red emission at indirect excitation. The results also showed that annealing process improved the crystal structure of ZnO nanosheets due to decrease of surface defects; however decreased ET and red emission because of diminishing in oxygen vacancy. In addition in ZnO nanorods sample with more surface area in comparison with ZnO nanosheets sample deep level emissions are enhanced.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2013

Improved microstructure of cement-based composites through the addition of rock wool particles

Rock wool is an inorganic fibrous substance produced by steam blasting and cooling molten glass. As with other industrial by-products, rock wool particles can be used as cementitious materials or ultra fine fillers in cement-based composites. This study investigated the microstructure of mortar specimens produced with cement-based composites that include various forms of rock wool particles. It conducted compressive strength testing, rapid chloride penetration tests, X-ray diffraction analysis, thermo-gravimetric analysis, and scanning electronic microscopy to evaluate the macro- and micro-properties of the cement-based composites. Test results indicate that inclusion of rock wool particles in composites improved compressive strength and reduced chloride ion penetration at the age of 91 days due to the reduction of calcium hydroxide content. Microscopic analysis confirms that the use of rock wool particles contributed to the formation of a denser, more compact microstructure within the hardened paste. In addition, X-ray diffraction analysis shows few changes in formation of pozzolanic reaction products and no new hydrations are formed with incorporating rock wool particles. - Highlights: • We report the microstructural characterization of cement-based composites. • Different mixes produced with various rock wool particles have been tested. • The influence of different mixes on macro and micro properties has been discussed. • The macro properties are included compressive strength and permeability. • XRD and SEM observations confirm the pozzolanic reaction in the resulting pastes.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Synthesis and electrocatalytic performance for p-nitrophenol reduction of rod-like Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites

Graphical abstract: The pure Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite with 5% Ag all exhibited rod-like morphology, and the microrods were actually composed of nanoparticles with mean size of 35 nm or so. - Highlights: • A facile route was designed to fabricate rod-like Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite nanomaterials. • Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite were modified on a GCE directly. • All samples exhibited enhanced catalytic property for p-nitrophenol reduction. - Abstract: Rod-like precursors of Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites with different Ag contents were synthesized via a co-precipitation method. Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composite samples were fabricated by calcining each precursor at 400 °C for 3 h. The as-prepared samples were characterized by thermogravimetric analysis and differential thermal gravimetric analysis (TGA/DTA), X-ray diffraction (XRD), transmission electron microscopy (TEM), and field emission scanning electron microscopy (FE-SEM), X-ray photoelectron spectroscopy (XPS), respectively. Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} composites were used as electrocatalyst modified on a glassy carbon electrode for p-nitrophenol reduction in basic solution. The results showed that p-nitrophenol could be reduced effectively on the modified electrode. By comparison with a bare glassy carbon electrode, peak current increased markedly with Co{sub 3}O{sub 4} and Ag/Co{sub 3}O{sub 4} samples, and peak potential decreased obviously with Ag/Co{sub 3}O{sub 4} samples. Ag/Co{sub 3}O{sub 4} composites with 4% Ag exhibited the highest electrocatalytic activity for p-nitrophenol reduction.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Fabrication of Au 25 (SG) 18 –ZIF-8 Nanocomposites: A Facile Strategy to Position Au 25 (SG) 18 Nanoclusters Inside and Outside ZIF-8

Multifunctional composite materials are currently highly desired for sustainable energy applications. A general strategy to integrate atomically precise Au 25 (SG) 18 with ZIF-8 (Zn(MeIm) 2 , MeIm = 2-methylimidazole), is developed in this paper via the typical Zn-carboxylate type of linkage. Au 25 (SG) 18 are uniformly encapsulated into a ZIF-8 framework (Au 25 (SG) 18 @ZIF-8) by coordination-assisted self-assembly. In contrast, Au 25 (SG) 18 integrated by simple impregnation is oriented along the outer surface of ZIF-8 (Au 25 (SG) 18 /ZIF-8). The porous structure and thermal stability of these nanocomposites are characterized by N 2 adsorption–desorption isothermal analysis and thermal gravimetric analysis. The distribution of Au 25 (SG) 18 in the two nanocomposites is confirmed by electron microscopy, and the accessibility of Au 25 (SG) 18 is evaluated by the 4-nitrophenol reduction reaction. The as-prepared nanocomposites retain the high porosity and thermal stability of the ZIF-8 matrix, while also exhibiting the desired catalytic and optical properties derived from the integrated Au 25 (SG) 18 nanoclusters (NCs). Au 25 (SG) 18 @ZIF-8 with isolated Au 25 sites is a promising heterogenous catalyst with size selectivity imparted by the ZIF-8 matrix. Finally, the structural distinction between Au 25 (SG) 18 @ZIF-8 and Au 25 (SG) 18 /ZIF-8 determines their different emission features, and provides a new strategy to adjust the optical behavior of Au 25 (SG) 18 for applications in bioimaging and biotherapy.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Effect of the hydration temperature on the microstructure of Class G cement: C-S-H composition and density

Curing temperature has a significant influence on cement paste microstructure and the properties of its principal hydrate C-S-H. In this paper, the effect of the hydration temperature in the range of 7 °C to 90 °C on the microstructure of a class G oil-well cement is studied. This is done by combining various experimental methods, including X-ray diffraction associated with the Rietveld analysis, thermo-gravimetric analysis, mercury intrusion porosimetry and porosity evaluation by drying. The experimental results show an increase of the capillary porosity and a decrease of the gel porosity by increasing the hydration temperature. This is attributed to a decrease of the C-S-H intrinsic porosity and a corresponding increase of the C-S-H density for higher curing temperatures. The experimental results are used in a simple analysis method to evaluate the density of C-S-H, as well as its C/S ratio and H/S ratio in dry and saturated conditions. The evaluated C-S-H density varies from 1.88 g/cm{sup 3} at 7 °C to 2.10 g/cm{sup 3} at 90 °C. The results also show a decrease of molar C/S ratio with increasing hydration temperature from 1.93 at 7 °C to 1.71 at 90 °C and of the H/S ratio from 5.1 at 7 °C to 2.66 at 90 °C.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Modification of Thermo-Mechanical Properties of Recycled PET by Vinyl Acetate (VAc) Monomer Grafting Using Gamma Irradiation

Vinyl acetate (VAc) monomer of different percentage was grafted onto the recycled polyethylene terephthalate (r-PET) films using gamma irradiation. The properties of these modified films were characterized by Fourier transform infrared spectroscopy (FTIR), mechanical properties testing (Tensile strength, Elongation at break), dynamic mechanical analysis (DMA) and thermo-gravimetric analysis (TGA). The Tensile Strength (TS) of the modified PET film increased by 132.25 % to the highest value of 50.12 MPa at 15% VAc monomer concentration at 3 kGy gamma dose, while the elongation at break (EB) decreased by 31.83 %. FTIR was used to investigate the molecular interaction of the modified films. TGA revealed that curve of the modified PET film shifted toward higher temperature region by 95 °C, which is very close to that of PET film made from virgin flakes. The results indicate that modified PET films of better mechanical and thermal properties were successfully prepared using VAc monomer grafting by gamma irradiation technique.

36 MATERIALS SCIENCE↗
DOE OSTI2017

Probing the oxidation kinetics of small permalloy particles

The oxidation of permalloys is important to apply in a wide range. The oxidation and diffusion mechanisms of small permalloy particles with different Fe content are studied by using thermal gravimetric analysis (TGA) and microstructure characterizations. Fe{sub 2}O{sub 3}/(Ni, Fe){sub 3}O{sub 4} plays a key role in the morphology evolution and diffusion mechanisms of small NiFe particles upon oxidation. The activation energies of grain boundary diffusion for the NiFe alloys increase from 141 kJ/mol to 208 kJ/mol as the Fe content increases from 0 to ~50 wt%. We have developed a diffusion process resolved temperature programed oxidation (PR-TPO) analysis method. Three diffusion mechanisms have been recognized by using this method: In addition to the grain boundary diffusion and lattice diffusion, our TGA analysis suggests that the phase conversion from Fe{sub 2}O{sub 3} to (Ni, Fe){sub 3}O{sub 4} induces diffusion change and affects the diffusion process at the intermediate temperature. Relevant oxidation kinetics and diffusion mechanisms are discussed. - Graphical abstract: The oxidation mechanisms of small Permalloy particles with different Fe content is studied by using thermal gravimetric analysis (TGA) and microstructure characterizations. The activation energies of grain boundary diffusion for the NiFe alloys increases from 140 kJ/mol to 208 kJ/mol as the Fe content increases from 0 to 50 wt% as determined by TGA. We have developed a diffusion process resolved temperature programed oxidation (DPR-TPO) analysis method, and three diffusion mechanisms have been recognized by using this method: In addition to the well-known grain boundary diffusion and lattice diffusion, we found that the phase conversion from Fe{sub 2}O{sub 3} to (Ni, Fe){sub 3}O{sub 4} will induce diffusion changes and affect the diffusion process at the intermediate temperature. The diffusion processes can be characterized by the corresponding characteristic peak temperatures in temperature programmed oxidation (TPO) analysis. This work not only give insight knowledge about the oxidation and diffusion processes of small permalloy particles, but also, provides a useful tool for analyzing solid-gas reactions of other materials. - Highlights: • The oxidation kinetics of small NiFe particles were studied by using thermoanalysis. • Grain boundary, lattice, and phase conversion induced diffusions were recognized. • The activation energy of oxidation increases with the Fe content in the alloy. • Each diffusion process corresponds to a characteristic temperature in TPO analysis. • NiFe alloys with ~5–10 wt% Fe content have the lowest oxidation rates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2016

Morphological, structural and thermal studies of gallium nitride ferrite

We report the synthesis and Characterization of III-V doped Nano ferrite Ga{sub (2x+2)}N Fe{sub 2(49-x)}O{sub 3} for x=1 and x=5 by Sol-Gel method. The Morphological, structural and Thermal characterisation studies are done by using Transmission Electron Microscopy, Energy Dispersive X-ray Analysis, Selected Area Electron Diffraction, Thermo-Gravimetric Analysis and Differential Thermal Analysis. Using the Sci-Finder software we could not trace any reports related to GaNFe{sub 2}O{sub 3} in the literature. It has been observed from our studies that the particles are in the Cylindrical and the Globular structure. The particle diameter values from the Histograms are in good agreement with the XRD values that were communicated by us earlier. The SAED and the EDAX studies reveal the confirmation of the composition and also that the synthesized Ferrite exhibits crystalline nature. The TG-DTA results show that the compound indicates constant sample weight.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2019

Effect Analysis of Nickel Ferrite (NiFe{sub 2}O{sub 4}) and Titanium Dioxide (TiO{sub 2}) Nanoparticles on CH{sub 4}/CO{sub 2} Gas Permeation Properties of Cellulose Acetate Based Mixed Matrix Membranes

Natural gas processing is very important industrial process. Major component of natural gas is methane, which is an increasingly utilized source of energy due to high thermal efficiency, while carbon dioxide act as an impurity and reduces its calorific value. In this research work, effects of nickel ferrite (NiFe{sub 2}O{sub 4}) and titanium dioxide (TiO{sub 2}) nanoparticles on the permeation properties of carbon dioxide (CO{sub 2}) and methane (CH{sub 4}) in cellulose acetate/polyethylene glycol (CA/PEG) membranes have been investigated. CA/PEG and CA/PEG based mixed matrix membranes (MMMs) are fabricated by using the solution casting method. Concentrations of TiO{sub 2} and NiFe{sub 2}O{sub 4} nanoparticles membranes are varied from 0 to 20 and 0 to 2 wt% respectively. Scanning electron microscope, tensile testing analysis, X-ray diffraction and thermal gravimetric analysis are used to characterize the fabricated membranes. Permeation study of these membranes has shown that in 5 wt%TiO{sub 2} MMMs, the permeability of CO{sub 2} and CH{sub 4} is increased up to 5.75 and 3.75 times as compared to pure polymer. By adding 1.5 wt% NiFe{sub 2}O{sub 4} in the polymer matrix, the permeability of CO{sub 2} and CH{sub 4} has improved up to 3.46 and 2.1 times as compared to pure polymer. It has been observed that the addition of inorganic nanoparticles in a polymer matrix helps to enhance the permeability of gases but it has little effect on CH{sub 4}/CO{sub 2} selectivity.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Buckling of Two-Dimensional Covalent Organic Frameworks under Thermal Stress

Two-dimensional covalent organic frameworks (2D COFs) are periodic, permanently porous, and lightweight solids that are polymerized from topologically designed monomers. The predictable design and structural modularity of these materials make them promising candidates for applications including catalysis, environmental remediation, chemical separations, and organic electronics, many of which will require stability to mechanical and thermal stress. Based on their reinforced structures and high degradation temperatures, as determined by thermal gravimetric analysis (TGA), many reports have claimed that COFs have excellent thermal stability. However, their stability to heat and pressure has not been probed using methods that report on structural changes rather than the loss of volatile compounds. Here, we explore two structurally analogous 2D COFs with different polymerization chemistries using in operando X-ray diffraction (XRD), which demonstrates the loss of crystallinity at lower temperatures than the degradation temperatures measured by TGA. Density functional theory calculations suggest that an asymmetric buckling of the COF lattice is responsible for the observed loss of crystallinity. In addition to their thermal stability, XRD of the 2D COFs under gas pressures up to 100 bar showed no loss in crystallinity or structural changes, indicating that these materials are robust to mechanical stress by applied pressure. We expect that these results will encourage further exploration of COF stability as a function of framework design and isolated form, which will guide the design of frameworks that withstand demanding application-relevant conditions.

Evans, Austin↗