Search NASA⌕ Search

SEARCH · Search NASA

Results for “differential thermal analysis”

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.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
NASA NTRS1990

Superconducting glass-ceramics in the Bi-Sr-Ca-Cu-O system

Differential thermal analysis, XRD, SEM, and resistivity measurements, have been used to study the recrystallization during various heat treatments of a Bi1.5SrCaCu2O(z) glass obtained by rapid quenching from the melt. Heating at 450 C formed the Bi(2+x)Sr(2-x)-CuO(z) solid solution designated 'R'. Between 765 and 845 C, R reacts slowly with the glass to form the 80 K superconductor Bi2(Sr,Ca)3Cu2O(z), together with CuO. Heating for 7 days at the higher temperature, followed by slow cooling, raised the temperature of zero resistance to 77 K.

De Guire, Mark R.↗
NASA NTRS1991

Crystallization and properties of Sr-Ba aluminosilicate glass-ceramic matrices

Powders of roller quenched (Sr,Ba)O-Al2O3-2SiO2 glasses of various compositions were uniaxially pressed into bars and hot isostatically pressed at 1350 C for 4 hours or cold isostatically pressed and sintered at different temperatures between 800 to 1500 C for 10 or 20 hours. Densities, flexural strengths, and linear thermal expansion were measured for three compositions. The glasss transition and crystallization temperatures were determined by Differential Scanning Calorimetry (DSC). The liquidus and crystallization temperature from the melt were measured using high temperature Differential Thermal Analysis (DTA). Crystalline phases formed on heat treatment of the glasses were identified by powder x ray diffraction. In Sr containing glasses, the monoclinic celsian phase always crystallized at temperatures above 1000 C. At lower temperatures, the hexagonal analog formed. The temperature for orthorhombic to hexagonal structure transformation increased monotonically with SrO content, from 327 C for BaO-Al2O3-2SiO2 to 758 C for SrO-Al2O3-2SiO2. These glass powders can be sintered to almost full densities and monoclinic celsian phase at a relatively low temperature of 1100 C.

Bansal, Narottam P.↗
NASA NTRS1991

Crystallization and properties of Sr-Ba aluminosilicate glass-ceramic matrices

Powders of roller quenched (Sr,Ba)O-Al2O3-2SiO2 glasses of various compositions were uniaxially pressed into bars and hot isostatically pressed at 1350 C for 4 hours or cold isostatically pressed and sintered at different temperatures between 800 to 1500 C for 10 or 20 hours. Densities, flexural strengths, and linear thermal expansion were measured for three compositions. The glass transition and crystallization temperatures were determined by Differential Scanning Calorimetry (DSC). The liquidus and crystallization temperature from the melt were measured using high temperature Differential Thermal Analysis (DTA). Crystalline phases formed on heat treatment of the glasses were identified by powder X ray diffraction. In Sr containing glasses, the monoclinic celsian phase always crystallized at temperatures above 1000 C. At lower temperatures, the hexagonal analog formed. The temperature for orthorhombic to hexagonal structural transformation increased monotonically with SrO content, from 327 C for BaO-Al2O3-2SiO2 to 758 C for SrO-Al2O3-2SiO2. These glass powders can be sintered to almost full densities and monoclinic celsian phase at a relatively low temperature of 1100 C.

Bansal, Narottam P.↗
NASA NTRS1992

Formation of a metastable ferromagnetic tau phase during containerless melt processing and rapid quenching in Mn-Al-C alloys

Solidification of selected Mn-Al-C alloys during containerless levitation and rapid quenching has yielded the first report for a ferromagnetic metastable tau phase formed directly from the melt. Complete solidification to tau phase was interrupted by the competitive evolution of an equilibrium epsilon phase during recalescence. The amount of undercooling required to produce the metastable ferromagnetic tau phase in a Mn(0.55)Al(0.433)C(0.017) alloy during solidification was estimated as approximately 470 K based on differential thermal analysis results. When the alloy carbon content was increased to 3.4 at. pct, transition in structure development occurred so that the samples exhibited gamma 2 phase formation as well as tau and epsilon phases.

Kim, Y. J.↗
NASA NTRS1992

Growth and characterization of lead bromide crystals

Lead(II) bromide was purified by a combination of directional freezing and zone-refining methods. Differential thermal analysis of the lead bromide showed that a destructive phase transformation occurs below the melting temperature. This transformation causes extensive cracking, making it very difficult to grow a large single crystal. Energy of phase transformation for pure lead bromide was determined to be 24.67 cal/g. To circumvent this limitation, crystals were doped by silver bromide which decreased the energy of phase transformation. The addition of silver helped in achieving the size, but enhanced the inhomogeneity in the crystal. The acoustic attenuation constant was almost identical for the pure and doped (below 3000 ppm) crystals.

Singh, N. B.↗
NASA NTRS1992

Studies on the reactive melt infiltration of silicon and silicon-molybdenum alloys in porous carbon

Investigations on the reactive melt infiltration of silicon and silicon-1.7 and 3.2 at percent molybdenum alloys into porous carbon preforms have been carried out by process modeling, differential thermal analysis (DTA) and melt infiltration experiments. These results indicate that the initial pore volume fraction of the porous carbon preform is a critical parameter in determining the final composition of the raction-formed silicon carbide and other residual phases. The pore size of the carbon preform is very detrimental to the exotherm temperatures due to liquid silicon-carbon reactions encountered during the reactive melt infiltration process. A possible mechanism for the liquid silicon-porous (glassy) carbon reaction has been proposed. The composition and microstructure of the reaction-formed silicon carbide has been discussed in terms of carbon preform microstructures, infiltration materials, and temperatures.

Singh, M.↗
NASA NTRS1993

Formation of a metastable ferromagnetic tau phase during containerless melt processing in Mn-Al-C alloys

This paper reports the production of a metastable ferromagnetic tau phase directly from the melt in Mn(0.55)Al(0.433)C(0.017), using a containerless processing method involving levitation melting followed by quenching. Using the results from differential thermal analysis measurements and an analysis of the phase equilibria, it was found that the minimum amount of undercooling level required for ferromagnetic metastable tau phase formation in this alloy was Delta T = 87 K. The attainment of this undercooling may be facilitated by the application of containerless melt processing.

Kim, Y. J.↗
NASA NTRS1993

Low temperature synthesis of monolithic transparent Ta2O5 gels from hydrolysis of metal alkoxide

Tantalum oxide gels in the form of transparent monoliths and powder were prepared from hydrolysis of tantalum pentaethoxide under controlled conditions using different mole ratios of Ta(OC2H5)5:C2H50H:H20:HCl. Alcohol acts as the mutual solvent and HCl as the deflocculating agent. For a fixed alkoxide:water:HCl ratio, time of gel formation increased with the alcohol to alkoxide mole ratio. Thermal evolution of the physical and structural changes in the gel was monitored by differential thermal analysis, thermogravimetric analysis, x-ray diffraction, and infrared spectroscopy. On heating to approximately 400 C, the amorphous gel crystallized into the low temperature orthorhombic phase Beta-Ta2O5, which transformed into the high temperature tetragonal phase Alpha-Ta2O5 when further heated to approximately 1450 C. The volume fraction of the crystalline phase increased with the firing temperature. The Alpha-Ta205 converted back into the low temperature phase, Beta-Ta2O5, on slow cooling through the transformation temperature of 1360 C indicating a slow but reversible transformation.

Bansal, Narottam P.↗
NASA NTRS1993

Differential Scanning Calorimetry (DSC) for planetary surface exploration

Differential Scanning Calorimetry (DSC) is the quantitative measurement of the enthalpic response of a material to a systematic change in temperature. In practice, the heat flow into or outward from a sample is measured as the sample is heated or cooled at a carefully controlled rate. DSC superficially resembles, but is not the same as differential thermal analysis (DTA), which is the measurement of temperature differences between a sample and reference material as the pair is heated or cooled. The fundamental properties measured by DSC are enthalpies and temperatures of phase transitions and constant-pressure heat capacities. Depending on instrument design and the nature of the sample, high-quality DSC analyses can be obtained on only a few milligrams of solid materials. DSC requires direct contact with the sample and generally degrades, if not destroys, the sample as a consequence of heating. In laboratory applications, it is common to subject the gaseous effluent from the DSC to analysis by a separate evolved-gas analyzer (EGA).

Gooding, James L.↗
NASA NTRS1994

Kinetics of phase transformation in glass forming systems

The objectives of this research were to (1) develop computer models for realistic simulations of nucleation and crystal growth in glasses, which would also have the flexibility to accomodate the different variables related to sample characteristics and experimental conditions, and (2) design and perform nucleation and crystallization experiments using calorimetric measurements, such as differential scanning calorimetry (DSC) and differential thermal analysis (DTA) to verify these models. The variables related to sample characteristics mentioned in (1) above include size of the glass particles, nucleating agents, and the relative concentration of the surface and internal nuclei. A change in any of these variables changes the mode of the transformation (crystallization) kinetics. A variation in experimental conditions includes isothermal and nonisothermal DSC/DTA measurements. This research would lead to develop improved, more realistic methods for analysis of the DSC/DTA peak profiles to determine the kinetic parameters for nucleation and crystal growth as well as to assess the relative merits and demerits of the thermoanalytical models presently used to study the phase transformation in glasses.

Ray, Chandra S.↗
NASA NTRS1994

Reactive Melt Infiltration of Silicon-Niobium Alloys in Microporous Carbons

Studies of the reactive melt infiltration of silicon-niobium alloys in microporous carbon preforms prepared by the pyrolysis of a polymer precursor have been carried out using modeling, Differential Thermal Analysis (DTA), and melt infiltration. Mercury porosimetry results indicate a very narrow pore size distribution with virtually all the porosity within the carbon preforms open to infiltrants. The morphology and amount of the residual phases (niobium disilicide and silicon) in the infiltrated material can be tailored according to requirements by careful control of the properties (pore size and pore volume) of the porous carbon preforms and alloy composition. The average room temperature four-point flexural strength of a reaction-formed silicon carbide material (made by the infiltration of medium pore size carbon preform with Si - 5 at. % Nb alloy) is 290 +/- 40 MPa (42 +/- 6 ksi) and the fracture toughness is 3.7 +/- 0.3 MPa square root of m. The flexural strength decreases at high temperatures due to relaxation of residual thermal stresses and the presence of free silicon in the material.

Singh, M.↗
NASA NTRS1995

Reactive melt infiltration of silicon-molybdenum alloys into microporous carbon preforms

Investigations on the reactive melt infiltration of silicon-1.7 and 3.2 at.% molybdenum alloys into microporous carbon preforms have been carried out by modeling, differential thermal analysis (DTA), and melt infiltration experiments. These results indicate that the pore volume fraction of the carbon preform is a very important parameter in determining the final composition of the reaction-formed silicon carbide and the secondary phases. Various undesirable melt infiltration results, e.g. choking-off, specimen cracking, silicon veins, and lake formation, and their correlation with inadequate preform properties are presented. The liquid silicon-carbon reaction exotherm temperatures are influenced by the pore and carbon particle size of the preform and the compositions of infiltrants. Room temperature flexural strength and fracture toughness of materials made by the silicon-3.2 at.% molybdenum alloy infiltration of medium pore size preforms are also discussed.

Singh, M.↗
NASA NTRS1994

Development of Advanced Alloys using Fullerenes

Development of advanced alloys using fullerenes is currently underway to produce materials for use in the extravehicular mobility unit (EMU). These materials will be directed toward commercial usages as they are continually developed. Fullerenes (of which the most common is C(sub 60)) are lightweight, nanometer size, hollow molecules of carbon which can be dispersed in conventional alloy systems to enhance strength and reduce weight. In this research, fullerene interaction with aluminum is investigated and a fullerene-reinforced aluminum alloy is being developed for possible use on the EMU. The samples were manufactured using standard commercial approaches including powder metallurgy and casting. Alloys have been processed having 1.3, 4.0 and 8.0 volume fractions of fullerenes. It has been observed that fullerene dispersion is related to the processing approach and that they are stable for the processing conditions used in this research. Emphasis will be given to differential thermal analysis and wavelength dispersive analysis of the processed alloys. These two techniques are particularly useful in determining the condition of the fullerenes during and after processing. Some discussion will be given as to electrical properties of fullerene-reinforced materials. Although the aluminum and other advanced alloys with fullerenes are being developed for NASA and the EMU, the properties of these materials will be of interest for commercial applications where specific Dual-Use will be given.

Sims, J.↗
NASA NTRS1995

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.↗
NASA NTRS1996

Phase Diagram of HgTe -ZnTe Pseudobinary and Density, Heat Capacity, and Enthalphy of Mixing of Hg(sub 1-x)Zn(sub x)Te Pseudobinary Melts

In this article, the solidus temperatures of the Hg(sub 1-x) Zn(sub x)Te pseudobinary phase diagram for several compositions in the low x region were measured by differential thermal analysis and the HgTe-ZnTe pseudobinary phase diagram was constructed. The densities of two HgZnTe melts, x = 0.10 and 0.16, were determined by an in situ pycnometric technique in a transparent furnace over, respectively, 110 and 50 C ranges of temperature. The thermodynamic properties of the melts, such as the heat capacity and enthalpy of mixing, were calculated for temperatures between the liquidus and 1500 C by assuming an associated solution model for the liquid phase.

Su, Ching-Hua↗
NASA NTRS1996

Effect of Pt Doping on Nucleation and Crystallization in Li2O.2SiO2 Glass: Experimental Measurements and Computer Modeling

Heterogeneous nucleation and its effects on the crystallization of lithium disilicate glass containing small amounts of Pt are investigated. Measurements of the nucleation frequencies and induction times with and without Pt are shown to be consistent with predictions based on the classical nucleation theory. A realistic computer model for the transformation is presented. Computed differential thermal analysis data (such as crystallization rates as a function of time and temperature) are shown to be in good agreement with experimental results. This modeling provides a new, more quantitative method for analyzing calorimetric data.

Narayan, K. Lakshmi↗
NASA NTRS1996

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.↗
NASA NTRS2001

Detection of Soluble and Fixed NH4+ in Clay Minerals by DTA and IR Reflectance Spectroscopy : A Potential Tool for Planetary Surface Exploration

Nitrogen is an essential element for life. It is the only element among the six major biogenic elements, C, O, S, O, P, H, whose presence in the Martian soil has not been positively and directly established. We describe here a study assessing the ability to detect NH4 in soils by two methods: differential thermal analysis (DTA) and infrared (IR) reflectance spectroscopy. Four standard clay minerals (kaolinite, montmorillonite, illite and attapulgite) and an altered tephra sample from Mauna Kea were treated with NH4 in this study. Samples of the NH4-treated and leached clays were analyzed by DTA and infrared (IR) reflectance spectroscopy to quantify the delectability of soluble and sorbed/fixed NH4. An exotherm at 270-280 C was clearly detected in the DTA curves of NH4-treated (non-leached) samples. This feature is assigned to the thermal decomposition reaction of NH4. Spectral bands observed at 1.56, 2.05, 2.12, 3.06, 3.3, 3.5, 5.7 and 7.0 microns in the reflectance spectra of NH4-treated and leached samples are assigned to the sorbed/fixed ammonium in the clays. The montmorillonite has shown the most intense absorbance due to fixed ammonium among the leached samples in this study, as a result of its high cation sorption capacity. It is concluded that the presence of sorbed or fixed NH4 in clays may be detected by infrared (IR) reflectance or emission spectroscopy. Distinction between soluble and sorbed NH4 may be achieved through the presence or absence of several spectral features assigned to the sorbed NH4 moietyi and, specifically, by use of the 4.2 micrometer feature assigned to solution NH4. Thermal analyses furnish supporting evidence of ammonia in our study through detection of N released at temperatures of 270-330 C. Based on these results it is estimated that IR spectra measured from a rover should be able to detect ammonia if present above 20 mg NH4/g sample in the surface layers. Orbital IR spectra and thermal analyses measured on a rover may be able to detect ammonia in soils as well but at higher abundances. The spectral features at 3.06 and 7.0 microns due to bound NH4 in clays and altered Hawaiian tephra appear to be the most promising for detection by orbital spectrometers. If N species are present on Mars the sedimentary deposits may be the best regions to look for them.

Janice, Bishop↗