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All sourcesNASA NTRSDOE OSTI
NASA NTRS1996

Scanning Tunneling Microscopy Studies of Diamond Films and Optoelectronic Materials

We present a summary of the research, citations of publications resulting from the research and abstracts of such publications. We have made no inventions in the performance of the work in this project. The main goals of the project were to set up a Chemical Vapor Deposition (CVD) diamond growth system attached to an UltraHigh Vacuum (UHV) atomic resolution Scanning Tunneling Microscopy (STM) system and carry out experiments aimed at studying the properties and growth of diamond films using atomic resolution UHV STM. We successfully achieved these goals. We observed, for the first time, the atomic structure of the surface of CVD grown epitaxial diamond (100) films using UHV STM. We studied the effects of atomic hydrogen on the CVD diamond growth process. We studied the electronic properties of the diamond (100) (2x1) surface, and the effect of alkali metal adsorbates such as Cs on the work function of this surface using UHV STM spectroscopy techniques. We also studied, using STM, new electronic materials such as carbon nanotubes and gold nanostructures. This work resulted in four publications in refereed scientific journals and five publications in refereed conference proceedings.

Perez, Jose M.↗
NASA NTRS1997

Effects of Fiber Coatings on Tensile Properties of Hi-Nicalon SiC/RBSN Tow Composites

Uncoated Hi-Nicalon silicon carbide (SiC) fiber tows and those coated with a single surface layer of pyrolytic boron nitride (PBN), double layers of PBN/Si-rich PBN, and boron nitride (BN)/SiC coatings deposited by chemical vapor deposition (CVD) method were infiltrated with silicon slurry and then exposed to N2, for 4 hr at 1200 and 1400 C. Room temperature ultimate tensile fracture loads and microstructural characterization of uncoated and CVD coated Hi-Nicalon SiC fiber reinforced reaction-bonded silicon nitride (RBSN) tow composites were measured to select suitable interface coating(s) stable under RBSN processing conditions. Results indicate that room temperature ultimate fracture loads of the uncoated Hi-Nicalon SiC/RBSN tow composites nitrided at both temperatures were significantly lower than those of the uncoated Hi-Nicalon tows without slurry infiltration. In contrast, all CVD coated Hi-Nicalon SiC/RBSN tow composites retained a greater fraction of the dry tow fracture load after nitridation at 1200 C, but degraded significantly after nitridation at 1400 C. Reaction between metal impurities (Fe and Ni) present in the attrition milled silicon powder and uncoated regions of SiC fibers appears to be the probable cause for fiber degradation.

Bhatt, Ramakrishna T.↗
NASA NTRS1999

Nutritional Aspects of Crewmembers' Cardiovascular Health Indicated by Dietary Lipids

This summer's project examined the relationships between dietary and physiological factors on serum lipoproteins using data from past United States astronauts. Nutritional assessment was required to determine whether a relationship existed between dietary intake and risk of cardiovascular disease (CVD) in crewmembers. Risk for CVD was assessed by the measurement of preflight, inflight, and postflight serum lipoproteins. The purpose of this project was to evaluate the dietary practices of past crewmembers before and during flight, and to examine their relationship with blood indicators of lipid status. Because of mortality and morbidity associated with CVD, such assessments are critical for the maintenance of astronaut health before, during, and after space flight. It was anticipated that the results from this project would assess the effects space flight and diet have on cardiovascular health, thus, defining the adequacy of the current dietary recommendations during space travel. It was hypothesized that the mean preflight serum lipoproteins compared to mean postflight serum lipoproteins would not be statistically different and that the current inflight diet is adequate in nutrient content, having little or no effect on lipoprotein levels.

Thurston, Marcelle A.↗
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 NTRS2000

Combinatorial Optimization of Heterogeneous Catalysts Used in the Growth of Carbon Nanotubes

Libraries of liquid-phase catalyst precursor solutions were printed onto iridium-coated silicon substrates and evaluated for their effectiveness in catalyzing the growth of multi-walled carbon nanotubes (MWNTs) by chemical vapor deposition (CVD). The catalyst precursor solutions were composed of inorganic salts and a removable tri-block copolymer (EO)20(PO)70(EO)20 (EO = ethylene oxide, PO = propylene oxide) structure-directing agent (SDA), dissolved in ethanol/methanol mixtures. Sample libraries were quickly assayed using scanning electron microscopy after CVD growth to identify active catalysts and CVD conditions. Composition libraries and focus libraries were then constructed around the active spots identified in the discovery libraries to understand how catalyst precursor composition affects the yield, density, and quality of the nanotubes. Successful implementation of combinatorial optimization methods in the development of highly active, carbon nanotube catalysts is demonstrated, as well as the identification of catalyst formulations that lead to varying densities and shapes of aligned nanotube towers.

Cassell, Alan M.↗
NASA NTRS1999

Measurements and Diagnostics of Diamond Films and Coatings

The commercial potential of chemical-vapor-deposited (CVD) diamond films has been established and a number of applications have been identified through university, industry, and government research studies. This paper discusses the methodologies used for property measurement and diagnostic of CVD diamond films and coatings. Measurement and diagnostic techniques studied include scanning electron microscopy, transmission electron microscopy, atomic force microscopy, stylus profilometry, x-ray diffraction, electron diffraction, Raman spectroscopy, Rutherford backscattering, elastic recoil spectroscopy, and friction examination. Each measurement and diagnostic technique provides unique information. A combination of techniques can provide the technical information required to understand the quality and properties of CVD diamond films, which are important to their application in specific component systems and environments. In this study the combination of measurement and diagnostic techniques was successfully applied to correlate deposition parameters and resultant diamond film composition, crystallinity, grain size, surface roughness, and coefficient of friction.

Miyoshi, Kazuhisa↗
NASA NTRS2001

Characterization of Carbon Nanotubes Grown by Chemical Vapor Deposition

Since the superior properties of multi-wall carbon nanotubes (MWCNT) could improve numerous devices such as electronics and sensors, many efforts have been made in investigating the growth mechanism of MWCNT to synthesize high quality MWCNT. Chemical vapor deposition (CVD) is widely used for MWCNT synthesis, and scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) are useful methods for analyzing the structure, morphology and composition of MWCNT. Temperature and pressure are two important growth parameters for fabricating carbon nanotubes. In MWCNT growth by CVD, the plasma assisted method is normally used for low temperature growth. However a high temperature environment is required for thermal CVD. A systematic study of temperature and pressure-dependence is very helpful to understanding MWCNT growth. Transition metal particles are commonly used as catalysis in carbon nanotube growth. It is also interesting to know how temperature and pressure affect the interface of carbon species and catalyst particles

Cochrane, J. C.↗
NASA NTRS2001

Preliminary Results of Field Emission Cathode Tests

Preliminary screening tests of field emission cathodes such as chemical vapor deposited (CVD) diamond, textured pyrolytic graphite, and textured copper were conducted at background pressures typical of electric thruster test facilities to assess cathode performance and stability. Very low power electric thrusters which provide tens to hundreds micronewtons of thrust may need field emission neutralizers that have a capability of tens to hundreds of microamperes. From current voltage characteristics, it was found that the CVD diamond and textured metals cathodes clearly satisfied the Fowler-Nordheim emission relation. The CVD diamond and a textured copper cathode had average current densities of 270 and 380 mA/sq cm, respectively, at the beginning-of-life. After a few hours of operation the cathode emission currents degraded by 40 to 75% at background pressures in the 10(exp -5) Pa to 10(exp -4) Pa range. The textured pyrolytic graphite had a modest current density at beginning-of-life of 84 mA/sq cm, but this cathode was the most stable of all. Extended testing of the most promising cathodes is warranted to determine if current degradation is a burn-in effect or whether it is a long-term degradation process. Preliminary experiments with ferroelectric emission cathodes, which are ceramics with spontaneous electric polarization, were conducted. Peak current densities of 30 to 120 mA/sq cm were obtained for pulse durations of about 500 ns in the 10(exp -4) Pa pressure range.

Sovey, James S.↗
NASA NTRS1999

Development of a Computational Chemical Vapor Deposition Model: Applications to Indium Nitride and Dicyanovinylaniline

A computational chemical vapor deposition (CVD) model is presented, that couples chemical reaction mechanisms with fluid dynamic simulations for vapor deposition experiments. The chemical properties of the systems under investigation are evaluated using quantum, molecular and statistical mechanics models. The fluid dynamic computations are performed using the CFD-ACE program, which can simulate multispecies transport, heat and mass transfer, gas phase chemistry, chemistry of adsorbed species, pulsed reactant flow and variable gravity conditions. Two experimental setups are being studied, in order to fabricate films of: (a) indium nitride (InN) from the gas or surface phase reaction of trimethylindium and ammonia; and (b) 4-(1,1)dicyanovinyl-dimethylaminoaniline (DCVA) by vapor deposition. Modeling of these setups requires knowledge of three groups of properties: thermodynamic properties (heat capacity), transport properties (diffusion, viscosity, and thermal conductivity), and kinetic properties (rate constants for all possible elementary chemical reactions). These properties are evaluated using computational methods whenever experimental data is not available for the species or for the elementary reactions. The chemical vapor deposition model is applied to InN and DCVA. Several possible InN mechanisms are proposed and analyzed. The CVD model simulations of InN show that the deposition rate of InN is more efficient when pulsing chemistry is used under conditions of high pressure and microgravity. An analysis of the chemical properties of DCVA show that DCVA dimers may form under certain conditions of physical vapor transport. CVD simulations of the DCVA system suggest that deposition of the DCVA dimer may play a small role in the film and crystal growth processes.

Cardelino, Carlos↗
NASA NTRS1998

Oxidation of Boron Nitride in Composites

Boron nitride (BN) is a prime candidate for fiber coatings in silicon carbide (SiC) fiber-reinforced SiC matrix composites. The properties of BN allow the fiber to impart beneficial composite properties to the matrix, even at elevated temperatures. The problem with BN is that it is readily attacked by oxygen. Although BN is an internal component of the composite, a matrix crack or pore can create a path for hot oxygen to attack the BN. This type of attack is not well understood. A variety of phenomena have been observed. These include borosilicate glass formation, volatilization of the BN, and under some conditions, preservation of the BN. In this study at the NASA Lewis Research Center, a series of BN materials and BN-containing model composites were methodically examined to understand the various issues dealing with the oxidation of BN in composites. Initial studies were done with a series of monolithic BN materials prepared by hot pressing and chemical vapor deposition (CVD). From these studies, we found that BN showed a strong orientation effect in oxidation and was extremely sensitive to the presence of water vapor in the environment. In addition, CVD material deposited at a high temperature showed much better oxidation behavior than CVD material deposited at a lower temperature.

Jacobson, Nathan S.↗
NASA NTRS2004

Improvement of thermal contact resistance by carbon nanotubes and nanofibers

Interfacial thermal resistance results of various nanotube and nanofiber coatings, prepared by chemical vapor deposition (CVD) methods, are reported at relatively low clamping pressures. The five types of samples examined include multi-walled and single-walled nanotubes growth by CVD, multi-walled nanotubes grown by plasma enhanced CVD (PECVD) and carbon nanofibers of differing aspect ratio grown by PECVD. Of the samples examined, only high aspect ratio nanofibers and thermally grown multi-walled nanotubes show an improvement in thermal contact resistance. The improvement is approximately a 60% lower thermal resistance than a bare Si-Cu interface and is comparable to that attained by commercially available thermal interface materials.

Evaluation Studies↗
NASA NTRS2005

Synthesizing Diamond from Liquid Feedstock

A relatively economical method of chemical vapor deposition (CVD) has been developed for synthesizing diamond crystals and films. Unlike prior CVD methods for synthesizing diamond, this method does not require precisely proportioned flows of compressed gas feedstocks or the use of electrical discharges to decompose the feedstocks to obtain free radicals needed for deposition chemical reactions. Instead, the feedstocks used in this method are mixtures of common organic liquids that can be prepared in advance, and decomposition of feedstock vapors is effected simply by heating. The feedstock used in this method is a solution comprising between 90 and 99 weight percent of methanol and the balance of one or more other oxyhydrocarbons that could include ethanol, isopropanol, and/or acetone. This mixture of compounds is chosen so that dissociation of molecules results in the desired proportions of carbon-containing radicals (principally, CH3) and of OH, H, and O radicals. Undesirably, the CVD temperature and pressure conditions thermodynamically favor the growth of graphite over the growth of diamond. The H radicals are desirable because they help to stabilize the growing surface of diamond by shifting the thermodynamic balance toward favoring the growth of diamond. The OH and O radicals are desirable because they preferentially etch graphite and other non-diamond carbon, thereby helping to ensure the net deposition of pure diamond. The non-methanol compounds are included in the solution because (1) methanol contains equal numbers of C and O atoms; (2) an excess of C over O is needed to obtain net deposition of diamond; and (3) the non-methanol molecules contain multiple carbon atoms for each oxygen atom and thus supply the needed excess carbon A typical apparatus used in this method includes a reservoir containing the feedstock liquid and a partially evacuated stainless-steel reaction chamber. The reservoir is connected to the chamber via tubing and a needle valve or other suitable flow controller. When the liquid enters the low-pressure environment inside the chamber, it evaporates to form a vapor mixture of the same chemical composition. In addition to the inlet for the feedstock liquid, the chamber is fitted with an outlet connected to a vacuum pump (not shown) through a throttle valve (also not shown) that is automatically controlled to keep the pressure at or near the required value throughout the deposition process. Inside the chamber, a spiral filament made of tungsten, tantalum, graphite, or other high-melting-temperature material is electrically heated to a temperature >2,000 C high enough to cause dissociation of vapor molecules into the aforementioned radicals. A deposition substrate typically, a diamond-polished silicon wafer about 2.5 cm square is positioned about 2 cm away from the filament. The exact location of the substrate is chosen so that the substrate becomes heated by the filament to a deposition temperature in the approximate range of 800 to 1,000 C.

Tzeng, Yonhua↗
NASA NTRS2004

Patterned Growth of Carbon Nanotubes or Nanofibers

A method and apparatus for the growth of carbon nanotubes or nanofibers in a desired pattern has been invented. The essence of the method is to grow the nanotubes or nanofibers by chemical vapor deposition (CVD) onto a patterned catalyst supported by a substrate. The figure schematically depicts salient aspects of the method and apparatus in a typical application. A substrate is placed in a chamber that contains both ion-beam sputtering and CVD equipment. The substrate can be made of any of a variety of materials that include several forms of silicon or carbon, and selected polymers, metals, ceramics, and even some natural minerals and similar materials. Optionally, the substrate is first coated with a noncatalytic metal layer (which could be a single layer or could comprise multiple different sublayers) by ion-beam sputtering. The choice of metal(s) and thickness(es) of the first layer (if any) and its sublayers (if any) depends on the chemical and electrical properties required for subsequent deposition of the catalyst and the subsequent CVD of the carbon nanotubes. A typical first-sublayer metal is Pt, Pd, Cr, Mo, Ti, W, or an alloy of two or more of these elements. A typical metal for the second sublayer or for an undivided first layer is Al at a thickness .1 nm or Ir at a thickness .5 nm. Proper choice of the metal for a second sublayer of a first layer makes it possible to use a catalyst that is chemically incompatible with the substrate. In the next step, a mask having holes in the desired pattern is placed over the coated substrate. The catalyst is then deposited on the coated substrate by ion-beam sputtering through the mask. Optionally, the catalyst could be deposited by a technique other than sputtering and/or patterned by use of photolithography, electron- beam lithography, or another suitable technique. The catalytic metal can be Fe, Co, Ni, or an alloy of two or more of these elements, deposited to a typical thickness in the range from 0.1 to 20 nm.

Delzeit, Lance D.↗
NASA NTRS2017

Cardiovascular Disease Risk in NASA Astronauts Across the Lifespan: Historical Cohort Studies

Acute effects of spaceflight on the cardiovascular system have been studied extensively, but the combined chronic effects of spaceflight and aging are not well understood. Preparation for and participation in space flight activities are potentially associated with cardiovascular disease risk factors (e.g., altered dietary and exercise habits, physical and emotional stress, circadian shifts, radiation). Further, astronauts who travel into space multiple times may be at an increased risk across their lifespan. However, comparing the risk of cardiovascular disease in astronauts to other large cohorts is difficult. For example, comparisons between astronauts and large national cohorts, such as the National Health and Nutrition Examination Survey and the National Health Information Survey, are hampered by significant differences in health status between astronauts and the general population, and most of these national studies fail to provide longitudinal data on population health. To address those limitations, NASA's Longitudinal Study of Astronaut Health previously sought to compare the astronauts to a cohort of civil servants employed at the Johnson Space Center. However, differences between the astronauts and civil servants at the beginning of the study, as well as differential follow up, limited the ability to interpret the results. To resolve some of these limitations, two unique cohorts of healthy workers, U.S. Air Force aviators and Cooper Center Longitudinal Study participants, have been identified as potential comparison populations for the astronaut corps. The Air Force cohort was chosen due to similarities in health at selection, screening, and some occupational exposures that Air Force aviators endure, many of which mirror that of the astronaut corps. The Cooper Clinic cohort, a generally healthy prevention cohort, was chosen for the vast array of clinical cardiovascular measures collected in a longitudinal manner complementary to those collected on astronauts, for a large number of subjects since 1971. The purpose of this study is to understand the incidence of cardiovascular disease outcomes and risk factors in the astronaut corps and determine whether the rates of disease are different than these two cohorts. The research questions are: 1. Are there differences in the incidence of CVD outcomes (MI, revascularization, and stroke) between each cohort and the NASA Astronaut cohort? 2. Are there differences in the incidence of CVD risks (hypertension, hyperlipidemia, arrhythmias, and diabetes) between each cohort and the NASA Astronaut cohort? 3. Are there differences between each cohort and the NASA Astronaut cohort in how CVD risk factors (e.g., lipids, behaviors) change across time? Collectively, results from these studies will enhance our understanding of how cardiovascular disease outcomes and risk factors change across time in astronauts compared to other longitudinally-studied healthy cohorts and determine if there are interactions between or additive effects of the occupational health effects of spaceflight exposure and normal aging.

Charvat, Jacqueline M.↗
NASA NTRS2018

Cardiovascular Disease Outcomes Among the NASA Astronaut Corps

BACKGROUND: Acute effects of spaceflight on the cardiovascular system have been studied extensively, but the combined chronic effects of spaceflight and aging are not well understood. Preparation for and participation in spaceflight activities are associated with changes in the cardiovascular system such as decreased carotid artery distensibility and decreased ventricular mass which may lead to an increased risk of cardiovascular disease. Additionally, astronauts who travel into space multiple times or for longer durations may be at an increased risk across their lifespan. To that end, the purpose of this study was to determine the incidence of common cardiovascular disease (CVD) outcomes among the NASA astronaut corps during their active career and through retirement. METHODS: Cardiovascular disease outcomes were defined as reports of any of the following: myocardial infarction (MI), revascularization procedures (coronary artery bypass graft surgery [CABG] or percutaneous coronary intervention [PCI]), hypertension, stroke or transient ischemic attack [TIA], heart failure, or total CVD (as defined by the AHA - combined outcome of MI, Angina Pectoris, heart failure, stroke, and hypertension). Each outcome was identified individually from review of NASA's Electronic Medical Record (EMR), EKG reports, and death certificates using ICD-9 codes as well as string searches of physician notes of astronaut exams that occurred between 1959 and 2016. RESULTS: Of 338 NASA astronauts selected as of 2016, 9 reported an MI, 12 reported a revascularization procedure, (7 PCI and 5 CABG), 4 reported Angina (without MI), 5 reported heart failure, 9 reported stroke/TIA, and 96 reported hypertension. Total CVD was reported in 105 astronauts. No astronaut who had an MI or revascularization procedure flew a spaceflight mission following the event. All MI, revascularization, and stroke events occurred in male astronauts. When reviewing astronaut ECG reports, abnormal ECG reports were found in only 8% of records (n=430) and mainly among retired astronauts (82%), with marked sinus bradycardia being the reason for the abnormal classification.

Charvat, Jacqueline M.↗
NASA NTRSDate not supplied

Evaluation of the spaceflight cardiovascular risk using the clinical prediction model Astro-CHARM and the NASA Radiation Risk Model

- Exposure to space radiation may pose a risk for cardiovascular diseases (CVD) during and after spaceflight. - The CVD risk should be quantified to plan future long-duration space missions such as the manned flight to Mars. - Assessing CVD risk is complicated by its multifactorial nature, where an individual’s risk is strongly influenced by risk factors such as family history, blood pressure, and lipid profiles. - In the NASA Space Radiation Risk Model, the metrics of radiation exposure-induced cases (REIC) and radiation exposure-induced death (REID) are used to quantify the risk attributable to radiation over a lifetime after exposure.

Ianik Plante↗
DOE OSTI2022

Particulates for additive manufacturing techniques

A method of making a particulate for an additive manufacturing technique includes receiving particulate at a chemical vapor deposition (CVD) reactor, flowing a hydrocarbon gas into the CVD reactor, decomposing the hydrocarbon gas in the CVD reactor, and depositing a carbonaceous coating on the particulate using a product of the decomposed hydrocarbon gas. The coating deposited over the particulate has a reflectivity that is lower than the reflectivity the underlying particulate body to reduce an energy input requirement for purposes of fusing the particulate into a layer of an article using an additive manufacturing technique. In embodiments, the coated particulate can be received at an additive manufacturing apparatus and fused into a layer of an article as a metallic-carbon composite using a high-density energy source.

42 ENGINEERING↗
DOE OSTI2022

Selected Area Deposition of PtC x Nanostructures: Implications for Functional Coatings of 3D Nanoarchitectures

Here, we report that selected area deposition of 3D nanostructures is induced via a pyrolytic laser chemical vapor deposition (CVD) process where selected area heating results from the unique photothermal transport regime that is intrinsic to 3D nanostructures. PtC x composite nanostructures were deposited by focused electron beam-induced deposition (FEBID) and used as 3D templates. Subsequent simultaneous localized delivery of an organometallic PtC x precursor and pulsed 915 nm laser irradiation to the pre-defined nanostructures results in selected area deposition on the FEBID features. Results indicate the ability to initiate the process on sub-diffraction-limit nanoscale features. To elucidate the mechanisms that are operative in the selected area deposition, we analyze the effects of the laser repetition rate, power, and pulse duration. Thermal simulations corroborate that the pseudo-1D thermal transport of the nanostructure geometry coupled with the optical and thermal properties of the nanostructure governs the CVD reaction. The results demonstrated here suggest that controlling the thermal transport in nanomaterial architectures could be a useful means to spatially control localized photothermally stimulated chemical reactions and induce selected area reactions.

36 MATERIALS SCIENCE↗