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NASA NTRS2011

Development of Meandering Winding Magnetometer (MWM (Register Trademark)) Eddy Current Sensors for the Health Monitoring, Modeling and Damage Detection of High Temperature Composite Materials

The increased use of high-temperature composite materials in modern and next generation aircraft and spacecraft have led to the need for improved nondestructive evaluation and health monitoring techniques. Such technologies are desirable to improve quality control, damage detection, stress evaluation and temperature measurement capabilities. Novel eddy current sensors and sensor arrays, such as Meandering Winding Magnetometers (MWMs) have provided alternate or complimentary techniques to ultrasound and thermography for both nondestructive evaluation (NDE) and structural health monitoring (SHM). This includes imaging of composite material quality, damage detection and .the monitoring of fiber temperatures and multidirectional stresses. Historically, implementation of MWM technology for the inspection of the Space Shuttle Orbiter Reinforced Carbon-Carbon Composite (RCC) leading edge panels was developed by JENTEK Sensors and was subsequently transitioned by NASA as an operational pre and post flight in-situ inspection at the Kennedy Space Center. A manual scanner, which conformed'automatically to the curvature of the RCC panels was developed and used as a secondary technique if a defect was found during an infrared thermography screening, During a recent proof of concept study on composite overwrapped pressure vessels (COPV's), three different MWM sensors were tested at three orientations to demonstrate the ability of the technology to measure stresses at various fiber orientations and depths. These results showed excellent correlation with actual surface strain gage measurements. Recent advancements of this technology have been made applying MWM sensor technology for scanning COPVs for mechanical damage. This presentation will outline the recent advance~ in the MWM.technology and the development of MWM techniques for NDE and SHM of carbon wra~ped composite overwrapped pressure vessels (COPVs) including the measurement of internal stresses via a surface mounted sensor array. In addition, this paper will outline recent efforts to produce sensors capable of making real-time measurements at temperatures up to 850 C, and discuss previous results demonstrating capability to monitor carbon fiber temperature changes within a composite material.

Russell, Richard↗

NASA NTRS2012

Electrical Conductivity of Rocks and Dominant Charge Carriers: Thermally Activated Positive Holes - Part 1

The prevailing view in the geophysics community is that the electrical conductivity structure of the Earth's continental crust over the 5-35 km depth range can best be understood by assuming the presence of intergranular fluids and/or of intragranular carbon films. Based on single crystal studies of melt-grown MgO, magma-derived sanidine and anorthosite feldspars and upper mantle olivine, we present evidence for the presence of electronic charge carriers, which derive from peroxy defects that are introduced during cooling, under non-equilibrium conditions, through a redox conversion of pairs of solute hydroxyl arising from dissolution of H2O.The peroxy defects become thermally activated in a 2-step process, leading to the release of defect electrons in the oxygen anion sublattice. Known as positive holes and symbolized by h(dot), these electronic charge carriers are highly mobile. Chemically equivalent to O(-) in a matrix of O(2-) they are highly oxidizing. Being metastable they can exist in the matrix of minerals, which crystallized in highly reduced environments. The h(dot) are highly mobile. They appear to control the electrical conductivity of crustal rocks in much of the 5-35 km depth range.

Freund, Friedemann T.↗

NASA NTRSDate not supplied

Thin-Ply: Exploration and Manufacturing with Automated Fiber Placement

Abstract Highly repeatable and nearly defect-free fabrication of composite parts is critical to the success and widespread acceptance of composite materials. Through optimization using thin-ply materials, composite parts can be manufactured to be lighter and tailored more specifically to anticipated design loads than with standard prepreg materials alone. However, defects arising from the thin-ply manufacturing process are not always similar to defects found with standard tows. These new defects warrant evaluation. At NASA Langley Research Center, the manufacturing process parameters associated with automated fiber placement (AFP), a slit tape-based composite manufacturing process, were optimized for the use of a thin-ply prepreg carbon-epoxy material. Carbon-epoxy tows with areal weights of 30 g/m2 and 70 g/m2 were used in these manufacturing trials. The AFP process parameters of heater output, compaction force, tow feed rate, and tow tension were adjusted and optimized for successful manufacturing. This article documents an exploration of thin-ply fabrication on both flat and complex-shaped surfaces. Ultimately, aerospace-quality laminates were made from the 70-g/m2 material, but imperfections in the 30-g/m2 material itself and the fact that the AFP machine was not designed for such a thin material meant that more research and trials are required to obtain flight-quality 30-g/m2 laminates.

Carbon-expoxy↗

NASA NTRSDate not supplied

Exploration and Manufacturing with Automated Fiber Placement

Highly repeatable and nearly defect-free fabrication of composite parts is critical to the success and widespread acceptance of composite materials. Through optimization using thin-ply materials, composite parts can be manufactured to be lighter and tailored more specifically to anticipated design loads than with standard prepreg materials alone. However, defects arising from the thin-ply manufacturing process are not always similar to defects found with standard tows. These new defects warrant evaluation. At NASA Langley Research Center, the manufacturing process parameters associated with automated fiber placement (AFP), a slit tape-based composite manufacturing process, were optimized for the use of a thin-ply prepreg carbon-epoxy material. Carbon-epoxy tows with areal weights of 30 g/m2 and 70 g/m2 were used in these manufacturing trials. The AFP process parameters of heater output, compaction force, tow feed rate, and tow tension were adjusted and optimized for successful manufacturing. This article documents an exploration of thin-ply fabrication on both flat and complex-shaped surfaces. Ultimately, aerospace-quality laminates were made from the 70-g/m2 material, but imperfections in the 30-g/m2 material itself and the fact that the AFP machine was not designed for such a thin material meant that more research and trials are required to obtain flight-quality 30-g/m2 laminates.

carbon-epoxy↗

NASA NTRS1999

Production and Characterization of Carbon Nanotubes and Nanotube-Based Composites

The Nobel Prize winning discovery of the Buckuball (C60) in 1985 at Rice University by a group including Dr. Richard Smalley led to the whole new class of carbon allotropes including fullerenes and nanotubes. Especially interesting from many viewpoints are single-walled carbon nanotubes, which structurally are like a single graphitic sheet wrapped around a cylinder and capped at the ends. This cylinders have diameter as small as 0.5 - 2 nm (1/100,000th the diameter of a human hair) and are as long as 0.1 - 1 mm. Nanotubes are really individual molecules and believed to be defect-free, leading to high tensile strength despite their low density. Additionally, these fibers exhibit electrical conductivity as high as copper, thermal conductivity as high as diamond, strength 100 times higher than steel at one-sixth the weight, and high strain to failure. Thus it is believed that developments in the field of nanotechnology will lead to stronger and lighter composite materials for next generation spacecraft. Lack of a bulk method of production is the primary reason nanotubes are not used widely today. Toward this goal JSC nanotube team is exploring three distinct production techniques: laser ablation, arc discharge and chemical vapor deposition (CVD, in collaboration with Rice University). In laser ablation technique high-power laser impinges on the piece of carbon containing small amount of catalyst, and nanotubes self-assemble from the resulting carbon vapor. In arc generator similar vapor is created in arc discharge between carbon electrodes with catalyst. In CVD method nanotubes grow at much lower temperature on small catalyst particles from carbon-containing feedstock gas (methane or carbon monoxide). As of now, laser ablation produces cleanest material, but mass yield is rather small. Arc discharge produces grams of material, but purity is low. CVD technique is still in baby steps, but preliminary results look promising, as well as perspective of scaling the process up. We are also working on necessary purification of nanotubes. Applications of nanotubes are in such various fields as lightweight composites, molecular electronics, energy storage (electrodes in Li ion batteries), flat panel displays, conductive polymers, etc. JSC nanotube team is focused on development of lightweight materials. We work on the injection thermoset epoxies reinforced with nanotubes. Early results show good wetting of nanotube surface with epoxy, which is very important. More research will be possible as more nanotubes become available.

Nikolaev, Pavel↗

NASA NTRS1985

Oxygen and carbon in silicon

The properties of the early transistors were determined by the minority-carrier lifetime, as is the silicon photovoltaic solar cell. Most of the devices on the modern integrated circuits are majority carrier devices, in part to avoid this lifetime dependence. The micro-electronics industry typically starts with wafers with a minority-carrier lifetime of 1000 micro-seconds, but during device fabrication this lifetime is reduced to beflow 1 micro-second, in spite of extraordinary cleanliness and precautions. Process-induced defects (PID) include point defects, defect complexes, line defects, and bulk precipitates. One of the aspects that needs to be better understood is the nature of minority carrier recombination at line defects and at precipitates. Some of the PIDs are known to be related to the fast-diffusers of the iron-series transition elements. One of the common techniques of dealing with these elements is intrinsic gettering by the oxygen precipitates. But even in the gettered state, there may be a residual effect on the lifetime. Oxygen is an almost ubiquitous impurity in silicon and plays an important role in both integrated circuits and solar cells. The isolated oxygen interstitial is electrically inactive, but in its various aggregated forms it has a variety of electrical activities. The agglomeration and precipitation of oxygen, including impurity gettering and the complicating role of carbon, is discussed.

Corbett, J. W.↗

NASA NTRS1995

The growth of cubic silicon carbide on a compliant substrate

Research has shown that silicon carbide grown on silicon and 6H silicon carbide has problems associated with these substrates. This is because silicon and silicon carbide has a 20% lattice mismatch and cubic silicon carbide has not been successfully achieved on 6H silicon carbide. We are investigating the growth of silicon carbide on a compliant substrate in order to grow defect free silicon carbide. This compliant substrate consists of silicon/silicon dioxide with 1200 A of single crystal silicon on the top layer. We are using this compliant substrate because there is a possibility that the silicon dioxide layer and the carbonized layer will allow the silicon lattice to shrink or expand to match the lattice of the silicon carbide. This would improve the electrical properties of the film for the use of device fabrication. When trying to grow silicon carbide, we observed amorphous film. To investigate, we examined the process step by step using RHEED. RHEED data showed that each step was amorphous. We found that just by heating the substrate in the presence of hydrogen it changed the crystal structure. When heated to 1000 C for 2 minutes, RHEED showed that there was an amorphous layer on the surface. We also heated the substrate to 900 C for 2 minutes and RHEED data showed that there was a deterioration of the single crystalline structure. We assumed that the presence of oxygen was coming from the sides of the silicon dioxide layer. Therefore, we evaporated 2500 A of silicon to all four edges of the wafer to try to enclose the oxygen. When heating the evaporated wafer to 900 C the RHEED data showed single crystalline structure however at 1000 C the RHEED data showed deterioration of the single crystalline structure. We conclude that the substrate itself is temperature dependent and that the oxygen was coming from the sides of the silicon dioxide layer. We propose to evaporate more silicon on the edges of the wafer to eliminate the escape of oxygen. this will allow us to grow single crystal cubic silicon carbide.

Mitchell, Sharanda↗

NASA NTRS2007

STS-114 Micrometeoroid/Orbital Debris (MMOD) Post-Flight Assessment

NASA Johnson Space Center (JSC) personnel assisted Kennedy Space Center (KSC) inspection teams in the identification of 41 micrometeoroid/orbital debris (MMOD) impact sites on the OV-103 vehicle (Discovery) during STS-114 postflight inspections. There were 14 MMOD impacts reported on the crew module windows (Figure 1). The largest impact feature, a 6.6 mm x 5.8 mm crater on window #4, was caused by a particle with an estimated diameter of 0.22 mm (Figure 2). This impact was among the largest ever recorded on a crew module window. The window was removed and replaced. Scanning Electron Microscope/Energy Dispersive X-ray (SEM/EDX) analysis of dental mold samples from the impact site to determine particle origin was inconclusive, possibly due to contamination picked up on the ferry flight from Edwards Air Force Base to KSC. The radiators on the inside of the payload bay doors sustained 19 impacts (Figure 3) with one of the impacts causing a face sheet perforation. The 0.61 mm diameter hole was produced by a particle with an estimated diameter of 0.4 mm, which approaches the 0.5-mm critical particle diameter of the wing leading edge reinforced carbon-carbon (RCC) panel high-temperature regions (Zone 3, Figure 4) that was established during Return to Flight testing of the RCC panels. An inspection of the payload bay door exterior insulation (FRSI) revealed a 5.8 mm x 4.5 mm defect that was caused by an MMOD particle with unknown composition, as the sample obtained was contaminated. Figure 5 provides a summary of the exterior surface survey that was conducted following the STS-114 mission. Two windows were removed and replaced due to hypervelocity impact. Nineteen impacts were recorded on the payload bay door radiators, with one face sheet penetration. Three impact sites were identified on the FRSI. There were four hypervelocity impact sites detected on the wing leading edge RCC panels. One impact was detected on the top cover of the TPS sample box (TSB) payload that was mounted on a carrier in the aft portion of the payload bay.

Hyde, J.↗

NASA NTRS2004

Process for Making Single-Domain Magnetite Crystals

A process for making chemically pure, single-domain magnetite crystals substantially free of structural defects has been invented as a byproduct of research into the origin of globules in a meteorite found in Antarctica and believed to have originated on Mars. The globules in the meteorite comprise layers of mixed (Mg, Fe, and Ca) carbonates, magnetite, and iron sulfides. Since the discovery of the meteorite was announced in August 1996, scientists have debated whether the globules are of biological origin or were formed from inorganic materials by processes that could have taken place on Mars. While the research that led to the present invention has not provided a definitive conclusion concerning the origin of the globules, it has shown that globules of a different but related chemically layered structure can be grown from inorganic ingredients in a multistep precipitation process. As described in more detail below, the present invention comprises the multistep precipitation process plus a subsequent heat treatment. The multistep precipitation process was demonstrated in a laboratory experiment on the growth of submicron ankerite crystals, overgrown by submicron siderite and pyrite crystals, overgrown by submicron magnesite crystals, overgrown by submicron siderite and pyrite. In each step, chloride salts of appropriate cations (Ca, Fe, and Mg) were dissolved in deoxygenated, CO2- saturated water. NaHCO3 was added as a pH buffer while CO2 was passed continuously through the solution. A 15-mL aliquot of the resulting solution was transferred into each of several 20 mL, poly(tetrafluoroethylene)-lined hydrothermal pressure vessels. The vessels were closed in a CO2 atmosphere, then transferred into an oven at a temperature of 150 C. After a predetermined time, the hydrothermal vessels were removed from the oven and quenched in a freezer. Supernatant solutions were decanted, and carbonate precipitates were washed free of soluble salts by repeated decantations with deionized water.

Golden, D. C.↗

NASA NTRS1979

Manufacture of low carbon astroloy turbine disk shapes by hot isostatic pressing. Volume 2, project 1

The performance of a hot isotatic pressed disk installed in an experimental engine and exposed to realistic operating conditions in a 150-hour engine test and a 1000 cycle endurance test is documented. Post test analysis, based on visual, fluorescent penetrant and dimensional inspection, revealed no defects in the disk and indicated that the disk performed satisfactorily.

Eng, R. D.↗

NASA NTRSDate not supplied

Carbon Nanotube – Polysiloxane Nanocomposites for Ablative Thermal Protection Systems

Ultra-high temperature resins (UHTR) such as polysiloxane possess excellent characteristics for ablation including low thermal conductivity, lightweight composition, high thermal resistance, and the ability to form a durable char layer. To enhance its mechanical strength, the aerospace industry utilizes fiber reinforcement, such as carbon fiber reinforced polysiloxane (CF-polysiloxane), due to its high strength-to-weight ratio. Carbon nanotubes (CNTs) have advantages over microfibers including higher specific strength, lower density, and customizable thermal conductivity. Their nano-scale dimensions allow for a more homogenous material compared to traditional microfibers. Conventional methods of incorporating CNTs into resins often have structural defects such as voids, CNT agglomerations, and randomly dispersed CNTs, resulting in marginal improvements in properties. A novel approach known as bulk nanocomposite laminating (BNL) has been introduced involving CNT densification, resin polymer infiltration, and pressurized curing to achieve a high packing density exceeding 35% by volume. Characterization and testing to simulate re-entry conditions is performed with a sample of CNT-polysiloxane nanocomposite cured onto a CF-polysiloxane backing. These samples are subjected to ablation by an oxyacetylene flame while collecting temperature data to evaluate thermal protection properties.

Palak B Patel↗

NASA NTRS2002

Efficient Nondestructive Evaluation of Prototype Carbon Fiber Reinforced Structures

Thermography and shearography methods of inspection rely on optic based technologies and can reduce the time and cost required to inspect composite tanks or aerostructures. Usually areas identified as suspect in the initial inspection results are reexamined with ultrasonic methods. This combination of techniques results in a rapid and comprehensive inspection of composite structures. Development of useful defect standards will be discussed. Examples of application of this inspection philosophy to prototype, GSE, and flight hardware will be presented. Methods organizing the inspection and evaluating the results will be considered.

Russell, Samuel S.↗

NASA NTRS1983

The growth of paracoccus halodenitrificans in a defined medium

A synthetic medium, consisting of inorganic salts and any of a number of carbon sources, supported the aerobic growth of Paracoccus halodenitrificans when supplemented with thiamine. The same medium plus a nitrogenous oxide supported anaerobic growth when additionally supplemented with methionine. The observation that vitamin B12 or betaine replaced methionine suggested that P. halodenitrificans had a defect in the cobalamin dependent pathway for methionine biosynthesis, as well as the inability to synthesize betaine when growing anaerobically.

Hochstein, L. I.↗

NASA NTRS1984

The growth of Paracoccus halodenitrificans in a defined medium

Hochstein, L. I.↗

NASA NTRS1988

Use of propane as a quench gas in argon-filled proportional counters and comparison with other quench gases

An experimental investigation of propane and six other quench gases was carried out in argon-filled proportional counters. The objective of the study was to find the best gas mixture for optimizing the gas gain and the energy resolution as well as to understand the role of the ionization potential of quench gases in determining these parameters. It was found that the best gas gains and energy resolutions are obtained with propane, ethane, and isobutane in that order. The ionization potentials of these three lie below the argon metastable potentials and have the lowest value of resonance defect compared to the other quench gases. The better results obtained with these mixtures can be explained by an increased ionization yield resulting from the Penning effect. Propylene and trans-2-butene give inferior performance compared to the above three gases. Methane and carbon dioxide, the most commonly used quench gases in the argon-filled detectors, provide the worst results.

Agrawal, P. C.↗

NASA NTRS2014

Nondestructive Evaluation Techniques for Development and Characterization of Carbon Nanotube Based Superstructures

Recently, multiple commercial vendors have developed capability for the production of large-scale quantities of high-quality carbon nanotube sheets and yarns. While the materials have found use in electrical shielding applications, development of structural systems composed of a high volume fraction of carbon nanotubes is still lacking. A recent NASA program seeks to address this by prototyping a structural nanotube composite with strength-toweight ratio exceeding current state-of-the-art carbon fiber composites. Commercially available carbon nanotube sheets, tapes, and yarns are being processed into high volume fraction carbon nanotube-polymer nanocomposites. Nondestructive evaluation techniques have been applied throughout this development effort for material characterization and process control. This paper will report on the progress of these efforts, including magnetic characterization of residual catalyst content, Raman scattering characterization of nanotube diameter, defect ratio, and nanotube strain, and polarized Raman scattering for characterization of nanotube alignment.

Wincheski, Buzz↗

NASA NTRS1998

Feasibility Assessment of Thermal Barrier Seals for Extreme Transient Temperatures

The assembly joints of modem solid rocket motor cases are generally sealed using conventional O-ring type seals. The 5500+ F combustion gases produced by rocket motors are kept a safe distance away from the seals by thick layers of phenolic insulation. Special compounds are used to fill insulation gaps leading up to the seals to prevent a direct flowpath to them. Design criteria require that the seals should not experience torching or charring during operation, or their sealing ability would be compromised. On limited occasions, NASA has observed charring of the primary O-rings of the Space Shuttle solid rocket nozzle assembly joints due to parasitic leakage paths opening up in the gap-fill compounds during rocket operation. NASA is investigating different approaches for preventing torching or charring of the primary O-rings. One approach is to implement a braided rope seal upstream of the primary O-ring to serve as a thermal barrier that prevents the hot gases from impinging on the O-ring seals. This paper presents flow, resiliency, and thermal resistance for several types of NASA rope seals braided out of carbon fibers. Burn tests were performed to determine the time to burn through each of the seals when exposed to the flame of an oxyacetylene torch (5500 F), representative of the 5500 F solid rocket motor combustion temperatures. Rope seals braided out of carbon fibers endured the flame for over six minutes, three times longer than solid rocket motor burn time. Room and high temperature flow tests are presented for the carbon seals for different amounts of linear compression. Room temperature compression tests were performed to assess seal resiliency and unit preloads as a function of compression. The thermal barrier seal was tested in a subscale "char" motor test in which the seal sealed an intentional defect in the gap insulation. Temperature measurements indicated that the seal blocked 2500 F combustion gases on the upstream side with very little temperature rise on the downstream side.

Steinetz, Bruce M.↗

NASA NTRS2017

Thermal Inspection of a Composite Fuselage Section Using a Fixed Eigenvector Principal Component Analysis Method

A composite fuselage aircraft forward section was inspected with flash thermography. The fuselage section is 24 feet long and approximately 8 feet in diameter. The structure is primarily configured with a composite sandwich structure of carbon fiber face sheets with a Nomex(Trademark) honeycomb core. The outer surface area was inspected. The thermal data consisted of 477 data sets totaling in size of over 227 Gigabytes. Principal component analysis (PCA) was used to process the data sets for substructure and defect detection. A fixed eigenvector approach using a global covariance matrix was used and compared to a varying eigenvector approach. The fixed eigenvector approach was demonstrated to be a practical analysis method for the detection and interpretation of various defects such as paint thickness variation, possible water intrusion damage, and delamination damage. In addition, inspection considerations are discussed including coordinate system layout, manipulation of the fuselage section, and the manual scanning technique used for full coverage.

Zalameda, Joseph N.↗