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Jacobson, Nathan S.

Publications and source records attributed to Jacobson, Nathan S..

At least 37 records · Page 2

Nondestructive Evaluation (NDE) for Characterizing Oxidation Damage in Cracked Reinforced Carbon-Carbon

In this study, coated reinforced carbon-carbon (RCC) samples of similar structure and composition as that from the NASA space shuttle orbiter's thermal protection system were fabricated with slots in their coating simulating craze cracks. These specimens were used to study oxidation damage detection and characterization using nondestructive evaluation (NDE) methods. These specimens were heat treated in air at 1143 C and 1200 C to create cavities in the carbon substrate underneath the coating as oxygen reacted with the carbon and resulted in its consumption. The cavities varied in diameter from approximately 1 to 3mm. Single-sided NDE methods were used because they might be practical for on-wing inspection, while X-ray micro-computed tomography (CT) was used to measure cavity sizes in order to validate oxidation models under development for carbon-carbon materials. An RCC sample having a naturally cracked coating and subsequent oxidation damage was also studied with X-ray micro-CT. This effort is a follow-on study to one that characterized NDE methods for assessing oxidation damage in an RCC sample with drilled holes in the coating.

Roth, Don J.↗

The Active Oxidation of Silicon Carbide

The high temperature oxidation of silicon carbide occurs in two very different modes. Passive oxidation forms a protective oxide film which limits further attack of the SiC: SiC(s) + 3/2 O2(g) = SiO2(s) + CO(g) Active oxidation forms a volatile oxide and may lead to extensive attack of the SiC: SiC(s) + O2(g) = SiO(g) + CO(g) Generally passive oxidation occurs at higher oxidant pressures and active oxidation occurs at lower oxidant pressures and elevated temperatures. Active oxidation is a concern for reentry, where the flight trajectory involves the latter conditions. Thus the transition points and rates of active oxidation are a major concern. Passive/active transitions have been studied by a number of investigators. An examination of the literature indicates many questions remain regarding the effect of impurity, the hysteresis of the transition (i.e. the difference between active-to-passive and passive-toactive), and the effect of total pressure. In this study we systematically investigate each of these effects. Experiments were done in both an alumina furnace tube and a quartz furnace tube. It is known that alumina tubes release impurities such as sodium and increase the kinetics in the passive region [1]. We have observed that the active-to-passive transition occurs at a lower oxygen pressure when the experiment is conducted in alumina tubes and the resultant passive silica scale contains sodium. Thus the tests in this study are conducted in quartz tubes. The hysteresis of the transition has been discussed in the detail in the original theoretical treatise of this problem for pure silicon by Wagner [2], yet there is little mention of it in subsequent literature. Essentially Wagner points out that the active-to-passive transition is governed by the criterion for a stable Si/SiO2 equilibria and the passive-to-active transition is governed by the decomposition of the SiO2 film. A series of experiments were conducted for active-to-passive and passive-to-active transitions by increasing and decreasing oxygen pressure, respectively. For pure silicon a dramatic difference was found; whereas for SiC the difference was not as great. This may be due to the oxidation of the carbon in SiC which may break down the scale [3]. The third area is the effect of total pressure. In the literature, low oxygen potentials are achieved via either low total pressure or low oxygen pressure in an O2/Ar mixture. Both types of experiments are done in this study and the differences are discussed with regard to the presence or absence of a boundary layer.

Jacobson, Nathan S.↗

Nondestructive Evaluation (NDE) for Characterizing Oxidation Damage in Cracked Reinforced Carbon-Carbon (RCC)

In this study, coated reinforced carbon-carbon (RCC) samples of similar structure and composition as that from the NASA space shuttle orbiter's thermal protection system were fabricated with slots in their coating simulating craze cracks. These specimens were used to study oxidation damage detection and characterization using nondestructive evaluation (NDE) methods. These specimens were heat treated in air at 1143 and 1200 C to create cavities in the carbon substrate underneath the coating as oxygen reacted with the carbon and resulted in its consumption. The cavities varied in diameter from approximately 1 to 3 mm. Single-sided NDE methods were used since they might be practical for on-wing inspection, while x-ray micro-computed tomography (CT) was used to measure cavity sizes in order to validate oxidation models under development for carbon-carbon materials. An RCC sample having a naturally-cracked coating and subsequent oxidation damage was also studied with x-ray micro-CT. This effort is a follow-on study to one that characterized NDE methods for assessing oxidation damage in an RCC sample with drilled holes in the coating.

Roth, Don J.↗

Oxidation Through Coating Cracks of SiC-Protected Carbon/Carbon

The oxidation of SiC-protected carbon/carbon through machined slots and naturally occurring craze cracks in the SiC was studied. The slot and crack geometries were characterized, and the subsurface oxidation of the carbon/carbon substrate at temperatures of 1000 to 1300 C in air was assessed using weight change, x-ray computed tomography, and optical microscopy of sections. Rate constants were derived from these measurements and compared with a two-step diffusion control model of carbon oxidation. Oxidation kinetic measurements on both the specimens with machined slots and with naturally occurring craze cracks showed good agreement with the model.

Jacobson, Nathan S.↗

Oxidation Through Coating Cracks of SiC-Protected Carbon/Carbon

The oxidation of SiC-protected carbon/carbon through machined slots and naturally occurring craze cracks in the SiC was studied. The slot and crack geometries were characterized, and the subsurface oxidation of the carbon/carbon substrate at temperatures of 1000 to 1300 C in air was assessed using weight change, x-ray computed tomography, and optical microscopy of sections. Rate constants were derived from these measurements and compared with a two-step diffusion control model of carbon oxidation. Oxidation kinetic measurements on both the specimens with machined slots and with naturally occurring craze cracks showed good agreement with the model.

Jacobson, Nathan S.↗

Oxidation Through Coating Cracks of SiC-Protected Carbon/Carbon

The oxidation of SiC-protected carbon/carbon through machined slots and naturally occurring craze cracks in the SiC was studied. The slot and crack geometries were characterized, and the subsurface oxidation of the carbon/carbon substrate at temperatures of 1000 to 1300 C in air was assessed using weight change, x-ray computed tomography, and optical microscopy of sections. Rate constants were derived from these measurements and compared with a two-step diffusion control model of carbon oxidation. Oxidation kinetic measurements on both the specimens with machined slots and with naturally occurring craze cracks showed good agreement with the model.

Jacobson, Nathan S.↗

Oxidation Microstructure Studies of Reinforced Carbon/Carbon

Laboratory oxidation studies of reinforced carbon/carbon (RCC) are discussed with particular emphasis on the resulting microstructures. This study involves laboratory furnace (500-1500 C deg) and arc-jet exposures (1538 C deg) on various forms of RCC. RCC without oxidation protection oxidized at 800 and 1100 C deg exhibits pointed and reduced diameter fibers, due to preferential attack along the fiber edges. RCC with a SiC conversion coating exhibits limited attack of the carbon substrate at 500, 700 and 1500 C deg. However samples oxidized at 900, 1100, and 1300 C deg show small oxidation cavities at the SiC/carbon interface below through-thickness cracks in the SiC coating. These cavities have rough edges with denuded fibers and can be easily distinguished from cavities created in processing. Arc-jet tests at 1538 C deg show limited oxidation attack when the SiC coating and glass sealants are intact. When the SiC/sealant protection system is damaged, attack is extensive and proceeds through matrix cracks, creating denuded fibers on the edges of the cracks. Even at 1538 C deg, where diffusion control dominates, attack is non-uniform with fiber edges oxidizing in preference to the bulk fiber and matrix.

Jacobson, Nathan S.↗

Analysis of Carbon/Carbon Fragments From the Columbia Tragedy

The extensive investigation following the Space Shuttle Orbiter Columbia accident of February 1, 2003 determined that hot gases entered the wing through a breach in the protective reinforced carbon/carbon (RCC) leading edge. In the current study, the exposed edges of the recovered RCC from the vicinity of the breach are examined with scanning electron microscopy and Raman spectroscopy. Electron microscopy of the exposed edges revealed regions of pointed carbon fibers, characteristic of exposure to high temperature oxidizing gases. The Raman technique relates the observed 1350 and 1580 to 1600 cm(-1) bands to graphitic dom ains and their corresponding temperatures of formation. Some of the regions showed evidence of exposure temperatures beyond 2700 ?C during the accident.

Tallant, David R.↗

Followup to Columbia Investigation: Reinforced Carbon/Carbon From the Breach Location in the Wing Leading Edge Studied

Initial estimates on the temperature and conditions of the breach in the Space Shuttle Columbia's wing focused on analyses of the slag deposits. These deposits are complex mixtures of the reinforced carbon/carbon (RCC) constituents, insulation material, and wing structural materials. Identification of melted/solidified Cerachrome insulation (Thermal Ceramics, Inc., Augusta, GA) indicated that the temperatures at the breach had exceeded 1760 C.

Jacobson, Nathan S.↗

Thermodynamics of Volatile Species in the Silicon-Oxygen-Hydrogen System Studied

The volatilization of silica (SiO2) to silicon hydroxides and oxyhydroxides because of reaction with water vapor is important in a variety of high-temperature corrosion processes. For example, the lifetimes of silicon carbide (SiC) and silicon nitride (Si3N4) - based components in combustion environments are limited by silica volatility. To understand and model this process, it is essential to have accurate thermodynamic data for the formation of volatile silicon hydroxides and oxyhydroxides.

Jacobson, Nathan S.↗

Materials Chemistry Issues in the Development of a Single-Crystal Solar/Thermal Refractive Secondary Concentrator

A translucent crystal concentrates and transmits energy to a heat exchanger, which in turn heats a propellant gas, working gas of a dynamic power system, or a thermopile. Materials are the limiting issue in such a system. Central is the durability of the crystal, which must maintain the required chemical, physical/optical, and mechanical properties as it is heated and cooled. This report summarizes available data to date on the materials issues with this system. We focus on the current leading candidate materials, which are sapphire (Al2O3) for higher temperatures and silica (SiO2) for lower temperatures. We use data from thermochemical calculations; laboratory coupon tests with silica and sapphire; and system tests with sapphire. The required chemical properties include low-vapor pressure and interfacial stability with supporting structural materials. Optical properties such as transmittance and index of refraction must be maintained. Thermomechanical stability is a major challenge for a large, single-crystal ceramic and has been discussed in another report. In addition to the crystal, other materials in the proposed system include refractory metals (Nb, Ta, Mo, W, and Re), carbon (C), and high-temperature ceramic insulation. The major issue here is low levels of oxygen, which lead to volatile refractory metal oxides and rapid consumption of the refractory metal. Interfacial reactions between the ceramic crystal and refractory metal are also discussed. Finally, high-temperature ceramic insulating materials are also likely to be used in this system. Outgassing is a major issue for these materials. The products of outgassing are typically reactive with the refractory metals and must be minimized.

Jacobson, Nathan S.↗

Performance of Ceramics in Severe Environments

Ceramics are generally stable to higher temperatures than most metals and alloys. Thus the development of high temperature structural ceramics has been an area of active research for many years. While the dream of a ceramic heat engine still faces many challenges, niche markets are developing for these materials at high temperatures. In these applications, ceramics are exposed not only to high temperatures but also aggressive gases and deposits. In this chapter we review the response of ceramic materials to these environments. We discuss corrosion mechanisms, the relative importance of a particular corrodent, and, where available, corrosion rates. Most of the available corrosion information is on silicon carbide (SIC) and silicon nitride (Si3N4) monolithic ceramics. These materials form a stable film of silica (SO2) in an oxidizing environment. We begin with a discussion of oxidation of these materials and proceed to the effects of other corrodents such as water vapor and salt deposits. We also discuss oxidation and corrosion of other ceramics: precurser derived ceramics, ceramic matrix composites (CMCs), ceramics which form oxide scales other than silica, and oxide ceramics. Many of the corrosion issues discussed can be mitigated with refractory oxide coatings and we discuss the current status of this active area of research. Ultimately, the concern of corrosion is loss of load bearing capability. We discuss the effects of corrosive environments on the strength of ceramics, both monolithic and composite. We conclude with a discussion of high temperature wear of ceramics, another important form of degradation at high temperatures.

Jacobson, Nathan S.↗

As-Fabricated Reinforced Carbon/Carbon Characterized

Reinforced carbon/carbon (RCC) is a critical material for the space shuttle orbiter. It is used on the wing leading edge and the nose cap, where maximum temperatures are reached on reentry. The existing leading-edge system is a single-plate RCC composite construction with a wall thickness of approximately 1/4 in., making it a prime reliant protection scheme for vehicle operation.

Jacobson, Nathan S.↗

Thermodynamics of the Si-O-H System

Thermodynamic functions for Si(OH)4(g) and SiO(OH)2(g) have been measured using the transpiration method. A second law enthalpy of formation and entropy and a third law enthalpy of formation has been calculated for Si(OH)4. The results are in very good agreement with previous experimental measurements, ab-initio calculations, and estimates.

Jacobson, Nathan S.↗

The Influence of Tungsten on the Chemical Composition of a Temporally Evolving Nanostructure of a Model Ni-Al-Cr Superalloy

The influence of W on the temporal evolution of gamma' precipitation toward equilibrium in a model Ni-Al-Cr alloy is investigated by three-dimensional atom-probe (3DAP) microscopy and transmission electron microscopy (TEM). We report on the alloys Ni-10 Al-8.5 Cr (at.%) and Ni-10 Al-8.5 Cr-2 W (at.%), which were aged isothermally in the gamma + gamma' two-phase field at 1073 K, for times ranging from 0.25 to 264 h. Spheroidal-shaped gamma' precipitates, 5-15 nm diameter, form during quenching from above the solvus temperature in both alloys at a high number density (approx. 10(exp 23/cu m). As gamma' precipitates grow with aging at 1073 K, a transition from spheriodal- to cuboidal-shaped precipitates is observed in both alloys. The elemental partitioning and spatially resolved concentration profiles across the gamma' precipitates are obtained as a function of aging time from three-dimensional atom-by-atom reconstructions. Proximity histogram concentration profiles of the quaternary alloy demonstrate that W concentration gradients exist in gamma' precipitates in the as-quenched and 0.25-h aging states, which disappear after 1 h of aging. The diffusion coefficient of W in gamma' is estimated to be 6.2 x 10(exp -20) sq m/s at 1073 K. The W addition decreases the coarsening rate constant, and leads to stronger partitioning of Al to gamma' and Cr to gamma.

Sudbrack, Chantal K.↗

Component Activity Measurements in the Ti-Al-O System by Knudsen Cell Mass Spectrometry

Titanium-aluminides (containing (alpha)2-Ti3Al and gamma-TiAl intermetallic phases) have received continued research focus due to their potential as low-density materials for structural applications at intermediate temperatures. However their application above about 850C is hindered by poor oxidation resistance, characterized by the formation of a non-protective TiO2+Al2O3 scale and an oxygen-enriched subsurface zone. Consistent with this are measured titanium and aluminum activities in "oxygen-free" titanium-aluminides, which indicate Al2O3 is only stable for aluminum concentrations greater then 54 atom percent at 1373 K. However, the inability to form a protective Al2O3 scale is in apparent conflict with phase diagram studies, as experimental isothermal sections of the Ti-Al-O system show gamma-TiAl + alpha2-Ti3Al structures are in equilibrium only with Al2O3. The apparent resolution to this conflict lies in the inclusion of oxygen effects in the thermodynamic measurements

Copland, Evan↗

Studies Conducted of Sodium Carbonate Contaminant Found on the Wing Leading Edge and the Nose Cap of the Space Shuttle Orbiter

In early 2001, three of the space shuttle orbiters were found to have a sodium carbonate contaminant on the wing leading edge and nose cap. These parts are made of a reinforced carbon/carbon material protected by silicon carbide (SiC) and a glass coating. The glass coating is known as Type A and is primarily sodium silicate with particles of SiC. NASA Glenn Research Center's Environmental Durability Branch was asked to determine the chemistry of this deposit formation and assess any possible detrimental effects. At low temperatures, the reverse reaction is favorable. Previous studies of the corrosion of glass show that carbon dioxide in the presence of water does form sodium carbonate on sodium silicate glass (ref. 1). It is quite likely that a similar scenario exists for the orbiter wing leading edge. All three orbiters that formed sodium carbonate were exposed to rain. This formation of sodium carbonate was duplicated in the laboratory. The Type A glass, which coats the wing leading edge and nose cap, was made in a freestanding form and exposed to water in two separate experiments. In one set of experiments, the coating was placed in a petri dish filled with water. As the water evaporated, sodium carbonate formed. In another case, water was slowly dripped on the coating and sodium carbonate formed. The sodium carbonate was detected by chemical analysis and, in some cases, xray diffraction showed a hydrated sodium carbonate. The next step was to examine possible detrimental effects of this sodium carbonate. There are three likely scenarios for the sodium carbonate deposit: (1) it may be removed with a simple rinse, (2) it may remain and flow back into the Type A glass after heating during reentry, or (3) it may remain and flow onto unprotected SiC and/or other parts after heating during reentry. The effect of case 1 is to remove the Na2O constituent from the Type A glass, thus decreasing its effectiveness as a sealant. Even so, overall, it is probably the best approach and was used by the NASA Kennedy Space Center when the deposits were first observed. The effect of case 2 is minimal and would actually restore the the Type A glass to its composition before carbonate formation. However, the problem with allowing the carbonate to remain leads to the third scenario, the deposit flowing onto other parts. A series of tests were conducted on unprotected SiC, and minimal effects were found in the short-term, but other ceramic and metal parts could be damaged by the molten sodium carbonate and would require close monitoring.

Jacobson, Nathan S.↗

Multiple Knudsen Cell Configuration Improved for Alloy Activity Studies

Knudsen effusion mass spectrometry (KEMS) allows the simultaneous determination of the identity and pressure of vapor species in equilibrium with a condensed phase as a function of temperature. This information can be used to determine the thermodynamic properties of materials. The partial pressure of species j in the cell is related to the measured intensity of the ion k formed from j, I(sup +) less than SABjk, and the absolute temperature T, where S(sub jk) is the sensitivity factor.

Copland, Evan H.↗