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NASA NTRS2006

Cleaning Carbon Nanotubes by Use of Mild Oxygen Plasmas

Experiments have shown that it is feasible to use oxygen radicals (specifically, monatomic oxygen) from mild oxygen plasmas to remove organic contaminants and chemical fabrication residues from the surfaces of carbon nanotubes (CNTs) and metal/CNT interfaces. A capability for such cleaning is essential to the manufacture of reproducible CNT-based electronic devices. The use of oxygen radicals to clean surfaces of other materials is fairly well established. However, previously, cleaning of CNTs and of graphite by use of oxygen plasmas had not been attempted because both of these forms of carbon were known to be vulnerable to destruction by oxygen plasmas. The key to success of the present technique is, apparently, to ensure that the plasma is mild . that is to say, that the kinetic and internal energies of the oxygen radicals in the plasma are as low as possible. The plasma oxygen-radical source used in the experiments was a commercial one marketed for use in removing hydrocarbons and other organic contaminants from vacuum systems and from electron microscopes and other objects placed inside vacuum systems. In use, the source is installed in a vacuum system and air is leaked into the system at such a rate as to maintain a background pressure of .0.56 torr (.75 Pa). In the source, oxygen from the air is decomposed into monatomic oxygen by radio-frequency excitation of a resonance of the O2 molecule (N2 is not affected). Hence, what is produced is a mild (non-energetic) oxygen plasma. The oxygen radicals are transported along with the air molecules in the flow created by the vacuum pump. In the experiments, exposure to the oxygen plasma in this system was shown to remove organic contaminants and chemical fabrication residues from several specimens. Many high-magnification scanning electron microscope (SEM) images of CNTs were taken before and after exposure to the oxygen plasma. As in the example shown in the figure, none of these images showed evidence of degradation of CNT structures.

Petkov, Mihail↗

NASA NTRS2015

Clays and Carbonates in a Groundwater-Fed 3.8 Ga Martian Lake: Insights to Subsurface Habitability on Mars

On Earth, the deep biosphere remains a largely unexplored, but clearly important carbon reservoir. Results from some uplifted central peaks in craters on Mars indicate that substantial carbon was also present at depth and might have helped sustain a deep biosphere. In fact, many factors relevant to deep biosphere habitability are more favorable on Mars than on Earth (e.g. porosity of the crust, geothermal gradient). Future exploration of Mars should include landing sites where materials have been exhumed from depth by meteor impact or basins where subsurface fluids have emerged, carrying clues to subsurface habitability. One of the most astrobiologically interesting sites on Mars McLaughlin Crater, a 93 km-diameter impact crater that formed approximately 4 b.y. ago. On the floor of the crater is a stratigraphic section of subhorizontal, layered sedimentary rocks with strong spectroscopic evidence for Fe-rich clay minerals and Mg-rich carbonates, which we interpret as ancient lacustrine deposits. The fluids that formed these materials likely originated in the subsurface, based on the paucity of channels leading into the crater basin and the fact that this is one of the deepest basins on Mars - a good candidate to have experienced upwelling of subsurface fluids. Therefore, the deposits within McLaughlin crater provide insight into subsurface processes on Mars. In this presentation, we will discuss the habitability of the martian subsurface as well as the geology of McLaughlin Crater and the possibility to detect biomarkers at that site with a future landed mission.

Michalski, Joseph↗

NASA NTRS2018

Biaxial Braided Flared Cone Structural Analysis

Computed Tomography (CT) is a useful tool for performing structural analysis on polymer based materials due to its high precision and accuracy. CT data was taken of two flared cones made from carbon fiber and fiberglass. One of the flared cones is pictured below. The variation in braid angle throughout the part was measured using Avizo 3D modelling software while the variation in thickness throughout the part was determined using MATLAB. Samples of pictures from the process of each of these analyses are shown below. The overall goal of this analysis was to collect structural data relevant to future testing of the parts.

Computed Tomography↗

NASA NTRS2006

Nanotube Dispersions Made With Charged Surfactant

Dispersions (including monodispersions) of nanotubes in water at relatively high concentrations have been formulated as prototypes of reagents for use in making fibers, films, and membranes based on single-walled carbon nanotubes (SWNTs). Other than water, the ingredients of a dispersion of this type include one or more charged surfactant(s) and carbon nanotubes derived from the HiPco(TradeMark) (or equivalent) process. Among reagents known to be made from HiPco(TradeMark)(or equivalent) SWNTs, these are the most concentrated and are expected to be usable in processing of bulk structures and materials. Test data indicate that small bundles of SWNTs and single SWNTs at concentrations up to 1.1 weight percent have been present in water plus surfactant. This development is expected to contribute to the growth of an industry based on applied carbon nanotechnology. There are expected to be commercial applications in aerospace, avionics, sporting goods, automotive products, biotechnology, and medicine.

Kuper, Cynthia↗

NASA NTRS2005

Flexible, Carbon-Based Ohmic Contacts for Organic Transistors

A low-temperature process for fabricating flexible, ohmic contacts for use in organic thin-film transistors (OTFTs) has been developed. Typical drainsource contact materials used previously for OTFTs include (1) vacuum-deposited noble-metal contacts and (2) solution-deposited intrinsically conducting molecular or polymeric contacts. Both of these approaches, however, have serious drawbacks.

Brandon, Erik↗

NASA NTRS2008

CO2 Sensors Based on Nanocrystalline SnO2 Doped with CuO

Nanocrystalline tin oxide (SnO2) doped with copper oxide (CuO) has been found to be useful as an electrical-resistance sensory material for measuring the concentration of carbon dioxide in air. SnO2 is an n-type semiconductor that has been widely used as a sensing material for detecting such reducing gases as carbon monoxide, some of the nitrogen oxides, and hydrocarbons. Without doping, SnO2 usually does not respond to carbon dioxide and other stable gases. The discovery that the electrical resistance of CuO-doped SnO2 varies significantly with the concentration of CO2 creates opportunities for the development of relatively inexpensive CO2 sensors for detecting fires and monitoring atmospheric conditions. This discovery could also lead to research that could alter fundamental knowledge of SnO2 as a sensing material, perhaps leading to the development of SnO2-based sensing materials for measuring concentrations of oxidizing gases. Prototype CO2 sensors based on CuO-doped SnO2 have been fabricated by means of semiconductor-microfabrication and sol-gel nanomaterial-synthesis batch processes that are amendable to inexpensive implementation in mass production.

Xu, Jennifer C.↗

NASA NTRS1988

Statistical characterization of carbon phenolic prepreg materials, volume 1

The objective was to characterize several lots of materials used for carbon/carbon and carbon/phenol product manufacture. Volume one is organized into testing categories based on raw material of product form. Each category contains a discussion of the sampling plan, comments and observations on each test method utilized, and a summary of the results obtained each category.

Beckley, Don A.↗

NASA NTRS2010

Multidimensional Tests of Thermal Protection Materials in the Arcjet Test Facility

Many thermal protection system materials used for spacecraft heatshields have anisotropic thermal properties, causing them to display significantly different thermal characteristics in different directions, when subjected to a heating environment during flight or arcjet tests. This paper investigates the effects of sidewall heating coupled with anisotropic thermal properties of thermal protection materials in the arcjet environment. Phenolic Impregnated Carbon Ablator (PICA) and LI-2200 materials (the insulation material of Shuttle tiles) were used for this study. First, conduction-based thermal response simulations were carried out, using the Marc.Mentat finite element solver, to study the effects of sidewall heating on PICA arcjet coupons. The simulation showed that sidewall heating plays a significant role in thermal response of these models. Arcjet tests at the Aerodynamic Heating Facility (AHF) at NASA Ames Research Center were performed later on instrumented coupons to obtain temperature history at sidewall and various radial locations. The details of instrumentation and experimental technique are the prime focus of this paper. The results obtained from testing confirmed that sidewall heating plays a significant role in thermal response of these models. The test results were later used to verify the two-dimensional ablation, thermal response, and sizing program, TITAN. The test data and model predictions were found to be in excellent agreement

Agrawal, Parul↗

NASA NTRS2010

Multidimensional Testing of Thermal Protection Materials in the Arcjet Test Facility

Many thermal protection system materials used for spacecraft heatshields have anisotropic thermal properties, causing them to display significantly different thermal characteristics in different directions, when subjected to a heating environment during flight or arcjet tests. The anisotropic effects are enhanced in the presence of sidewall heating. This paper investigates the effects of anisotropic thermal properties of thermal protection materials coupled with sidewall heating in the arcjet environment. Phenolic Impregnated Carbon Ablator (PICA) and LI-2200 materials (the insulation material of Shuttle tiles) were used for this study. First, conduction-based thermal response simulations were carried out, using the Marc.Mentat finite element solver, to study the effects of sidewall heating on PICA arcjet coupons. The simulation showed that sidewall heating plays a significant role in thermal response of these models. Arcjet tests at the Aerodynamic Heating Facility (AHF) at NASA Ames Research Center were performed later on instrumented coupons to obtain temperature history at sidewall and various radial locations. The details of instrumentation and experimental technique are the prime focus of this paper. The results obtained from testing confirmed that sidewall heating plays a significant role in thermal response of these models. The test results were later used to validate the two-dimensional ablation, thermal response, and sizing program, TITAN. The test data and model predictions were found to be in excellent agreement

Agrawal, Parul↗

NASA NTRS2003

Investigation of Celestial Solid Analogs

Our far infrared studies of both hydrophobic and hydrophilic aerogel grains have demonstrated that the mm and sub-mm wave absorption produced by the fundamental two level systems (TLS) mechanism represents a more significant contribution for these open grain structures than for bulk amorphous silicate grains. We found that the region with the anomalous temperature dependence of the spectral index due to the TLS excitations can extend in a fluffy material up to 80 per cm, which is well beyond its typical upper limit for bulk glasses. Currently there is no theoretical explanation for this surprising result. The effects of reduced dimensionality on the optical properties of carbonaceous grains have been studied with a systematic investigation of carbon aerogels. This spectroscopic approach has permitted a more reliable determination of the single grain mass normalized absorption coefficient based on the experimentally determined characteristics of the fluffy material rather than on first principles calculations involving the bulk properties of the substance. Our finding is that the electrical connectivity of the material is the main factor affecting its far infrared absorption coefficient. Another one of the main constituents of the interstellar dust, amorphous ice, has been investigated in the mm-wave region both in the high (HDA) and low (LDA) density amorphous phases and as a function of impurities. We found that doping either phase with ionic (LiCl) or molecular (methanol) impurities decreases the difference in the mm-wave absorption coefficient between the HDA and LDA ice phases so that the HDA spectrum can be used as an analog for impure ice absorption in the far infrared spectral region.

Sievers, A. J.↗

NASA NTRS2012

Detection of Carbon Monoxide Using Polymer-Composite Films with a Porphyrin-Functionalized Polypyrrole

Post-fire air constituents that are of interest to NASA include CO and some acid gases (HCl and HCN). CO is an important analyte to be able to sense in human habitats since it is a marker for both prefire detection and post-fire cleanup. The need exists for a sensor that can be incorporated into an existing sensing array architecture. The CO sensor needs to be a low-power chemiresistor that operates at room temperature; the sensor fabrication techniques must be compatible with ceramic substrates. Early work on the JPL ElectronicNose indicated that some of the existing polymer-carbon black sensors might be suitable. In addition, the CO sensor based on polypyrrole functionalized with iron porphyrin was demonstrated to be a promising sensor that could meet the requirements. First, pyrrole was polymerized in a ferric chloride/iron porphyrin solution in methanol. The iron porphyrin is 5, 10, 15, 20-tetraphenyl-21H, 23Hporphine iron (III) chloride. This creates a polypyrrole that is functionalized with the porphyrin. After synthesis, the polymer is dried in an oven. Sensors were made from the functionalized polypyrrole by binding it with a small amount of polyethylene oxide (600 MW). This composite made films that were too resistive to be measured in the device. Subsequently, carbon black was added to the composite to bring the sensing film resistivity within a measurable range. A suspension was created in methanol using the functionalized polypyrrole (90% by weight), polyethylene oxide (600,000 MW, 5% by weight), and carbon black (5% by weight). The sensing films were then deposited, like the polymer-carbon black sensors. After deposition, the substrates were dried in a vacuum oven for four hours at 60 C. These sensors showed good response to CO at concentrations over 100 ppm. While the sensor is based on a functionalized pyrrole, the actual composite is more robust and flexible. A polymer binder was added to help keep the sensor material from delaminating from the electrodes, and carbon was added to improve the conductivity of the material.

Homer, Margie L.↗

NASA NTRS1994

A search for SiO, OH, CO and HCN radio emission from silicate-carbon stars

We report upper limits for radio emission of SiO at 86 and 43 GHz, of OH at 1612 and 1665/1667 MHz, of CO at 115 GHz and HCN at 88.6 GHz in the silicate-carbon stars. These upper limits of SiO imply that oxygen-rich material has not been detected within 2R(sub star) of a central star even though the detected emission from silicate dust grains, H2O and OH maser establishes the presence of oxygen-rich material from about tens to thousands of AU of a central star. The upper limit of the SiO abundance is consistent with that found in oxygen-rich envelopes. Upper limits of the mass loss rate (based on the CO data) are estimated to be between 10(exp -6) to 10(exp -7) solar mass/yr assuming a distance of 1.5 kpc for these stars. The absence of HCN microwave emission implies that no carbon-rich material can be detected at large distances (thousands of AU) from a central star. The lack of detections of SiO, CO, and HCN emission is most likely due to the large distances of these stars. A number of C stars were detected in CO and HCN, but only the M supergiant VX Sgr was detected in CO.

Little-Marenin, I. R.↗

NASA NTRS2012

Performance Characterization and Simulation of Amine-Based Vacuum Swing Sorption Units for Spacesuit Carbon Dioxide and Humidity Control

Controlling carbon dioxide (CO2) and water (H2O) vapor concentrations in a space suit is critical to ensuring an astronauts safety, comfort, and capability to perform extra-vehicular activity (EVA) tasks. Historically, this has been accomplished using lithium hydroxide (LiOH) and metal oxide (MetOx) canisters. Lithium hydroxide is a consumable material that requires priming with water before it becomes effective at removing carbon dioxide. MetOx is regenerable through a power-intensive thermal cycle but is significantly heavier on a volume basis than LiOH. As an alternative, amine-based vacuum swing beds are under aggressive development for EVA applications. The vacuum swing units control atmospheric concentrations of both CO2 and H2O through fully-regenerative process. The current concept, referred to as the rapid cycle amine (RCA), has resulted in numerous laboratory prototypes. Performance of these prototypes have been assessed experimentally and documented in previous reports. To support developmental e orts, a first principles model has also been established for the vacuum swing sorption technology. For the first time in several decades, a major re-design of Portable Life Support System (PLSS) for the extra-vehicular mobility unit (EMU) is underway. NASA at Johnson Space Center built and tested an integrated PLSS test bed of all subsystems under a variety of simulated EVA conditions of which the RCA prototype played a significant role. The efforts documented herein summarize RCA test performance and simulation results for single and variable metabolic rate experiments in an integrated context. In addition, a variety of off-nominal tests were performed to assess the capability of the RCA to function under challenging circumstances. Tests included high water production experiments, degraded vacuum regeneration, and deliberate valve/power failure and recovery.

Swickrath, Michael J.↗

NASA NTRS1992

Structural analysis of an NDE-inspected carbon-carbon component

In this research, it is demonstrated that the integration of nondestructive evaluation with the finite element method (a quantitative NDE/FEM approach) can be used for analysis and behavior prediction of advanced materials, such as fiber composites, after processing and during in-service testing. First, stress, strain, and energy data were calculated by the finite element method for square plates with a 10 percent difference in the material properties between specified segments, i.e., between the center and the outside section or between two halves of the plate. This demonstrated the efficiency of the method in predicting variations in the structural behavior based on small material property differences. Then, finite element analyses and actual axial compression tests were performed on a Space Shuttle brake stator made from woven carbon-carbon composites. The material properties used in the numerical modeling of the stator were previously characterized at a large number of points on the component by quantitative NDE-procedures, i.e., ultrasonics and radiography. The results from the experimental compressive loading tests were used to verify the NDE/FEM results. Good agreement was found for most parameters.

Striz, A. G.↗

NASA NTRS1991

The use of carboranes as oxidation inhibitors for carbon-carbon composites

Carbon-carbon composites have many beneficial properties for use in aerospace applications, including their high specific strength and modulus at elevated temperatures. However, they share with all carbon based substances a strong tendency to burn when heated in air. In order to exploit their good qualities, it is necessary to slow or prevent their oxidation during use. Molecular inhibiters offer protection with the advantage of being able to form a homogeneous solution with the resin. Since boron oxides are known to provide the desired kind of protection, molecular compounds based on boron seem reasonable candidates to test as inhibitors. Performance tests indicated that carboranes are excellent materials for obtaining high uniform loadings of boron inhibitors in glassy carbon materials and thus reducing their rates of oxidation. Further, there is evidence that the use of substituted derivatives could provide more complete and thorough forms of protection.

Petty, John T.↗

NASA NTRS1996

Design, Fabrication and Testing of Multilayer Coated X-Ray Optics for the Water Window Imaging X-Ray Microscope

Hoover et. al. built and tested two imaging Schwarzschild multilayer microscopes. These instruments were constructed as prototypes for the "Water Window Imaging X-Ray Microscope," which is a doubly reflecting, multilayer x-ray microscope configured to operate within the "water window." The "water window" is the narrow region of the x-ray spectrum between the K absorption edges of oxygen (lamda = 23.3 Angstroms) and of carbon (lamda = 43.62 Angstroms), where water is relatively highly transmissive and carbon is highly absorptive. This property of these materials, thus permits the use of high resolution multilayer x-ray microscopes for producing high contrast images of carbon-based structures within the aqueous physiological environments of living cells. We report the design, fabrication and testing of multilayer optics that operate in this regime.

Spencer, Dwight C.↗

NASA NTRS2013

Parametric Thermal Soak Model for Earth Entry Vehicles

The analysis and design of an Earth Entry Vehicle (EEV) is multidisciplinary in nature, requiring the application many disciplines. An integrated tool called Multi Mission System Analysis for Planetary Entry Descent and Landing or M-SAPE is being developed as part of Entry Vehicle Technology project under In-Space Technology program. Integration of a multidisciplinary problem is a challenging task. Automation of the execution process and data transfer among disciplines can be accomplished to provide significant benefits. Thermal soak analysis and temperature predictions of various interior components of entry vehicle, including the impact foam and payload container are part of the solution that M-SAPE will offer to spacecraft designers. The present paper focuses on the thermal soak analysis of an entry vehicle design based on the Mars Sample Return entry vehicle geometry and discusses a technical approach to develop parametric models for thermal soak analysis that will be integrated into M-SAPE. One of the main objectives is to be able to identify the important parameters and to develop correlation coefficients so that, for a given trajectory, can estimate the peak payload temperature based on relevant trajectory parameters and vehicle geometry. The models are being developed for two primary thermal protection (TPS) materials: 1) carbon phenolic that was used for Galileo and Pioneer Venus probes and, 2) Phenolic Impregnated Carbon Ablator (PICA), TPS material for Mars Science Lab mission. Several representative trajectories were selected from a very large trade space to include in the thermal analysis in order to develop an effective parametric thermal soak model. The selected trajectories covered a wide range of heatload and heatflux combinations. Non-linear, fully transient, thermal finite element simulations were performed for the selected trajectories to generate the temperature histories at the interior of the vehicle. Figure 1 shows the finite element model that was used for the simulations. The results indicate that it takes several hours for the thermal energy to soak into the interior of the vehicle and achieve maximum payload temperatures. In addition, a strong correlation between the heatload and peak payload container temperature is observed that will help establishing the parametric thermal soak model.

Agrawal, Parul↗

NASA NTRS2019

Challenges in Qualification of Thermal Protection Systems in Extreme Entry Environments

Planetary entry vehicles employ ablative TPS materials to shield the aeroshell from entry aeroheating environments. To ensure mission success, it must be demonstrated that the heat shield system, including local features such as seams, does not fail at conditions that are suitably margined beyond those expected in flight. Furthermore, its thermal response must be predictable, with acceptable fidelity, by computational tools used in heat shield design. Mission assurance is accomplished through a combination of ground testing and material response modelling. A material's robustness to failure is verified through arcjet testing while its thermal response is predicted by analytical tools that are verified against experimental data. Due to limitations in flight-like ground testing capability and lack of validated high-fidelity computational models, qualification of heat shield materials is often achieved by piecing together evidence from multiple ground tests and analytical simulations, none of which fully bound the flight conditions and vehicle configuration. Extreme heating environments (>2000 W/sq. cm heat flux and >2 atm pressure), experienced during entries at Venus, Saturn and Ice Giants, further stretch the current testing and modelling capabilities for applicable TPS materials. Fully-dense Carbon Phenolic was the material of choice for these applications; however, since heritage raw materials are no longer available, future uses of re-created Carbon Phenolic will require re-qualification. To address this sustainability challenge, NASA is developing a new dual-layer material based on 3D weaving technology called Heat shield for Extreme Entry Environments (HEEET). Regardless of TPS material, extreme environments pose additional certification challenges beyond what has been typical in recent NASA missions. Scope of this presentation: This presentation will give an overview of challenges faced in verifying TPS performance at extreme heating conditions. Examples include: (1) Bounding aeroheating parameters (heat flux, pressure, shear and enthalpy) in ground facilities. How to certify TPS if environments can't be bounded or aeroheating parameters can't be simultaneously achieved. (2) Higher uncertainties in ground test environments (facility calibration and analytical predictions) at extreme conditions. (3) Testing in flows similar to planetary atmosphere composition (H2/He for Gas and Ice Giants). (4) Test sample size limitations for qualifying seam designs. (5) Lack of computational tools capable of simulating all significant aspects of TPS performance (including initiation and propagation of failures). This presentation will provide recommendations on how the EDL community can address these challenges and mitigate some of the risks involved in flying TPS materials at extreme conditions. Examples include: (1) Dedicated activity to understanding TPS failure modes. Develop computational tools capable of modelling fluid interaction with material's thermostructural response. Validate these tools through failure testing. A better understanding of failure mechanisms may eliminate the need to fully bound all aeroheating parameters in ground testing. (2) Enhancements to current testing facilities to simulate flight-like ablation mechanism (ex. testing in Nitrogen at Ames Interaction Heating Facility to limit oxidation in favor of more sublimation). (3) Improved characterization of test conditions with new diagnostic methods and determination of environment uncertainty through rigorous statistical analysis of available data. (4) Design margin policies that are directly tied to uncertainties in ground test environments and modelling fidelity

Mahzari, Milad↗