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NASA NTRS2003

Diagnostics of Carbon Nanotube Formation in a Laser Produced Plume: An Investigation of the Metal Catalyst by Laser Ablation Atomic Fluorescence Spectroscopy

Carbon nanotubes, elongated molecular tubes with diameters of nanometers and lengths in microns, hold great promise for material science. Hopes for super strong light-weight material to be used in spacecraft design is the driving force behind nanotube work at JSC. The molecular nature of these materials requires the appropriate tools for investigation of their structure, properties, and formation. The mechanism of nanotube formation is of particular interest because it may hold keys to controlling the formation of different types of nanotubes and allow them to be produced in much greater quantities at less cost than is currently available. This summer's work involved the interpretation of data taken last summer and analyzed over the academic year. The work involved diagnostic studies of carbon nanotube formation processes occurring in a laser-produced plume. Laser ablation of metal doped graphite to produce a plasma plume in which carbon nanotubes self assemble is one method of making carbon nanotube. The laser ablation method is amenable to applying the techniques of laser spectroscopy, a powerful tool for probing the energies and dynamics of atomic and molecular species. The experimental work performed last summer involved probing one of the metal catalysts, nickel, by laser induced fluorescence. The nickel atom was studied as a function of oven temperature, probe laser wavelength, time after ablation, and position in the laser produced plume. This data along with previously obtained data on carbon was analyzed over the academic year. Interpretations of the data were developed this summer along with discussions of future work. The temperature of the oven in which the target is ablated greatly influences the amount of material ablated and the propagation of the plume. The ablation conditions and the time scale of atomic and molecular lifetimes suggest that initial ablation of the metal doped carbon target results in atomic and small molecular species. The metal atoms survive for several milliseconds while the gaseous carbon atoms and small molecules nucleate more rapidly. Additional experiments and the development of in situ methods for carbon nanotube detection would allow these results to be interpreted from the perspective of carbon nanotube formation.

deBoer, Gary↗
NASA NTRS2000

Plasticity and Kinky Chemistry of Carbon Nanotubes

Since their discovery in 1991, carbon nanotubes have been the subject of intense research interest based on early predictions of their unique mechanical, electronic, and chemical properties. Materials with the predicted unique properties of carbon nanotubes are of great interest for use in future generations of aerospace vehicles. For their structural properties, carbon nanotubes could be used as reinforcing fibers in ultralight multifunctional composites. For their electronic properties, carbon nanotubes offer the potential of very high-speed, low-power computing elements, high-density data storage, and unique sensors. In a continuing effort to model and predict the properties of carbon nanotubes, Ames accomplished three significant results during FY99. First, accurate values of the nanomechanics and plasticity of carbon nanotubes based on quantum molecular dynamics simulations were computed. Second, the concept of mechanical deformation catalyzed-kinky-chemistry as a means to control local chemistry of nanotubes was discovered. Third, the ease of nano-indentation of silicon surfaces with carbon nanotubes was established. The elastic response and plastic failure mechanisms of single-wall nanotubes were investigated by means of quantum molecular dynamics simulations.

Srivastava, Deepak↗
NASA NTRS2008

Control of the Diameter and Chiral Angle Distributions during Production of Single-wall Carbon Nanotubes

Many applications of single wall carbon nanotubes (SWCNT), especially in microelectronics, will benefit from use of certain (n,m) nanotube types (metallic, small gap semiconductor, etc.). However, as produced SWCNT samples are polydispersed, with many (n,m) types present and typical approximate 1:2 metal/semiconductor ratio. It has been recognized that production of SWCNTs with narrow 'tube type populations' is beneficial for their use in applications, as well as for the subsequent sorting efforts. In the present work, SWCNTs were produced by a pulsed laser vaporization (PLV) technique. The nanotube type populations were studied with respect to the production temperature with two catalyst compositions: Co/Ni and Rh/Pd. The nanotube type populations were measured via photoluminescence, UV-Vis-NIR absorption and Raman spectroscopy. It was found that in the case of Co/Ni catalyst, decreased production temperature leads to smaller average diameter, exceptionally narrow diameter distribution, and strong preference toward (8,7) nanotubes. The other nanotubes present are distributed evenly in the 7-30 deg chiral angle range. In the case of Rh/Pd catalyst, a decrease in the temperature leads to a small decrease in the average diameter, with the chiral angle distribution skewed towards 30 o and a preference toward (7,6), (8,6) and (8,7) nanotubes. However, the diameter distribution remains rather broad. These results demonstrate that PLV production technique can provide at least partial control over the nanotube (n,m) populations. In addition, these results have implications for the understanding the nanotube nucleation mechanism in the laser oven.

Nikolaev, Pavel↗
NASA NTRS2005

Gears Based on Carbon Nanotubes

Gears based on carbon nanotubes (see figure) have been proposed as components of an emerging generation of molecular- scale machines and sensors. In comparison with previously proposed nanogears based on diamondoid and fullerene molecules, the nanotube-based gears would have simpler structures and are more likely to be realizable by practical fabrication processes. The impetus for the practical development of carbon-nanotube- based gears arises, in part, from rapid recent progress in the fabrication of carbon nanotubes with prescribed diameters, lengths, chiralities, and numbers of concentric shells. The shafts of the proposed gears would be made from multiwalled carbon nanotubes. The gear teeth would be rigid molecules (typically, benzyne molecules), bonded to the nanotube shafts at atomically precise positions. For fabrication, it may be possible to position the molecular teeth by use of scanning tunneling microscopy (STM) or other related techniques. The capability to position individual organic molecules at room temperature by use of an STM tip has already been demonstrated. Routes to the chemical synthesis of carbon-nanotube-based gears are also under investigation. Chemical and physical aspects of the synthesis of molecular scale gears based on carbon nanotubes and related molecules, and dynamical properties of nanotube- based gears, have been investigated by computational simulations using established methods of quantum chemistry and molecular dynamics. Several particularly interesting and useful conclusions have been drawn from the dynamical simulations performed thus far: The forces acting on the gears would be more sensitive to local molecular motions than to gross mechanical motions of the overall gears. Although no breakage of teeth or of chemical bonds is expected at temperatures up to at least 3,000 K, the gears would not work well at temperatures above a critical range from about 600 to about 1,000 K. Gear temperature could probably be controlled by use of coolant gases. For a given application, the gears would work well at temperatures below the critical range, provided that the rotational energy was less than the energy required to tilt the teeth through an angle of 20 . The predominant mechanism of gear failure would be slippage caused by tilting of teeth. Gears would resume functioning if the slipping gears were decelerated sufficiently.

Jaffe, Richard↗
NASA NTRS2001

Future Nanotube Commercialization Opportunities at the NASA Marshall Space Flight Center and the US Army Aviation and Missile Command

Nanotube technology has broad applicability to programs at both the NASA Marshall Space Flight Center (MSFC) and the US Army Aviation and Missile Command (AMCOM). MSFC has interest in applications of nanotubes as sensors and high strength lightweight materials for propulsion system components, avionic systems, and scientific instruments. MSFC is currently pursuing internal programs to develop nanotube temperature sensors, heat pipes, and metal matrix composites. In support of these application areas MSFC is interested in growth of long nanotubes, growth of nanotubes in the microgravity environment, and nanotubes fabricated from high temperature materials such as Boron Nitride or Silicon Carbide. AMCOM is similarly interested in nanotube applications which take advantage of the nanotube thermal conductance properties, high strength, and lightweight. Applications of interest to AMCOM include rocket motor casing structures, rocket nozzles, and lightweight structure and aeronautic skins.

Watson, Michael↗
NASA NTRS2000

Modeling of Current-Voltage Characteristics in Large Metal-Semiconducting Carbon Nanotube Systems

A model is proposed for two observed current-voltage (I-V) patterns in recent experiment with a scanning tunneling microscope tip and a carbon nanotube [Collins et al., Science 278, 100 (1997)]. We claim that there are two contact modes for a tip (metal)-nanotube (semiconductor) junction depending whether the alignment of the metal and the semiconductor band structures is (1) variable (vacuum-gap) or (2) fixed (touching) with V. With the tip grounded, the tunneling case in (1) would produce large dI/dV with V > 0, small dI/dV with V < 0, and I = 0 near V = 0 for an either n- or p-nanotube. However, the Schottky mechanism in (2) would result in forward current with V < 0 for an n-nanotube, while with V > 0 for an p-nanotube. The two observed I-V patterns are thus entirely explained by a tip-nanotube contact of the two types, where the nanotube must be n-type. We apply this model to the source-drain I-V characteristics in a long nanotube-channel field-effect-transistor with metallic electrodes at low temperature [Zhou et al., Appl. Phys. Lett. 76, 1597 (2000)], and show that two independent metal-semiconductor junctions in series are responsible for the observed behavior.

Yamada, Toshishige↗
NASA NTRS2001

Metallic Electrode: Semiconducting Nanotube Junction Model

A model is proposed for two observed current-voltage (I-V) patterns in an experiment with a scanning tunneling microscope tip and a carbon nanotube [Collins et al., Science 278, 100 ('97)]. We claim that there are two contact modes for a tip (metal) -nanotube semi conductor) junction depending whether the alignment of the metal and semiconductor band structure is (1) variable (vacuum-gap) or (2) fixed (touching) with V. With the tip grounded, the tunneling case in (1) would produce large dI/dV with V > 0, small dI/dV with V < 0, and I = 0 near V = 0 for an either n- or p-nanotube. However, the Schottky mechanism in (2) would result in forward current with V < 0 for an n-nanotube, while with V > 0 for an p-nanotube. The two observed I-V patterns are thus entirely explained by a tip-nanotube contact of the two types, where the nanotube must be n-type. We apply this picture to the source-drain I-V characteristics in a long nanotube-channel field-effect-transistor (Zhou et al., Appl. Phys. Lett. 76, 1597 ('00)], and show that two independent metal-semiconductor junctions connected in series are responsible for the observed behavior.

Yamada, Toshishige↗
NASA NTRS2001

Formation of Carbon Nanotubes in a Microgravity Environment

Even though nanotube science has become one of the worlds most rapidly advancing areas of research, very little is known about the processes involved in nanotube synthesis. To study the formation of carbon nanotubes in an environment unhindered by the buoyancy induced flows generated by the high temperatures necessary to vaporize carbon and grow nanotubes, we have designed a miniature carbon arc apparatus that can produce carbon nanotubes under microgravity conditions. During the first phase of this project, we designed, built, and successfully tested the mini carbon arc in both 1g and 2.2 sec drop tower microgravity conditions. We have demonstrated that microgravity can eliminate the strong convective flows from the carbon arc and we have successfully produced single-walled carbon nanotubes in microgravity. We believe that microgravity processing will allow us to better understand the nanotube formation process and eventually allow us to grow nanotubes that are superior to ground-based production.

Alford, J. M.↗
NASA NTRS1999

Single Particle Transport Through Carbon Nanotube Wires: Effect of Defects and Polyhedral Cap

The ability to manipulate carbon nanotubes with increasing precision has enabled a large number of successful electron transport experiments. These studies have primarily focussed on characterizing transport through both metallic and semiconducting wires. Tans et al. demonstrated ballistic transport in single-wall nanotubes for the first time, although the experimental configuration incurred large contact resistance. Subsequently, methods of producing low contact resistances have been developed and two terminal conductances smaller than 50 k-ohms have been repeatably demonstrated in single-wall and multi-wall nanotubes. In multi-wall nanotubes, Frank et al. demonstrated a resistance of approximately h/2e(exp 2) in a configuration where the outermost layer made contact to a liquid metal. This was followed by the work of de Pablo et al. where a resistance of h(bar)/27e(exp 2) (approximately 478 ohms) was measured in a configuration where electrical contact was made to many layers of a multi-wall nanotube. Frank et al. and Pablo et al. note that each conducting layer contributes a conductance of only 2e(exp 2)/h, instead of the 4e(exp 2)/h that a single particle mode counting picture yields. These small resistances have been obtained in microns long nanotubes, making them the best conducting molecular wires to date. The large conductance of nanotube wires stems from the fact that the crossing bands of nanotubes are robust to defect scattering.

Anantram, M. P.↗
NASA NTRS1999

Anisotropic Plasticity of BN Nanotubes

Plastic collapse of compressed BN nanotubes are investigated and compared with carbon nanotubes of similar nature. Using a generalized tight-binding molecular dynamics (GTBMD) method for system containing B, N and C atoms we compute stiffness and plastic collapse of BN and C nanotubes under axial compression. For small compressional strain, BN nanotubes are found to be about 92% as stiff as similar C nanotubes. Due to BN bond buckling effect, however, the elastic limit of BN nanotubes is found to be more than C nanotubes. A route to plasticity is explored in which we find that at elastic limit the accumulated strain is released by a local plastic deformation of the nanotube. The mechanism of strain release and the resulting plastic deformation, however. are anisotropic in nature. The strain is released preferentially towards N as leading edge of a buckled BN bond and the tube, compressed at both ends, plastically collapses preferentially towards one end. Details of the anisotropic plasticity and prospective applications will be discussed in this presentation.

Madhu, Menon↗
NASA NTRS2002

Computational Nanomechanics of Carbon Nanotubes and Composites

Nanomechanics of individual carbon and boron-nitride nanotubes and their application as reinforcing fibers in polymer composites has been reviewed with interplay of theoretical modeling, computer simulations and experimental observations. The emphasis in this work is on elucidating the multi-length scales of the problems involved, and of different simulation techniques that are needed to address specific characteristics of individual nanotubes and nanotube polymer-matrix interfaces. Classical molecular dynamics simulations are shown to be sufficient to describe the generic behavior such as strength and stiffness modulus but are inadequate to describe elastic limit and nature of plastic buckling at large strength. Quantum molecular dynamics simulations are shown to bring out explicit atomic nature dependent behavior of these nanoscale materials objects that are not accessible either via continuum mechanics based descriptions or through classical molecular dynamics based simulations. As examples, we discus local plastic collapse of carbon nanotubes under axial compression and anisotropic plastic buckling of boron-nitride nanotubes. Dependence of the yield strain on the strain rate is addressed through temperature dependent simulations, a transition-state-theory based model of the strain as a function of strain rate and simulation temperature is presented, and in all cases extensive comparisons are made with experimental observations. Mechanical properties of nanotube-polymer composite materials are simulated with diverse nanotube-polymer interface structures (with van der Waals interaction). The atomistic mechanisms of the interface toughening for optimal load transfer through recycling, high-thermal expansion and diffusion coefficient composite formation above glass transition temperature, and enhancement of Young's modulus on addition of nanotubes to polymer are discussed and compared with experimental observations.

Srivastava, Deepak↗
NASA NTRS2002

Nanotube Sensors

Under this project, we explored the feasibility of utilizing carbon nanotubes in sensing applications. The grant primarily supported a graduate student, who worked on a number of aspects of the electrical properties of carbon nanotubes in collaboration with other researchers in my group. The two major research accomplishments are described below. The first accomplishment is the demonstration that solution carbon nanotube transistors functioned well in an electrolyte environment. This was important for two reasons. First, it allowed us to explore the ultimate limits of nanotube electronic performance by using the electrolyte as a highly effective gate, with a dielectric constant of approximately 80 and an effective insulator thickness of approximately 1 nm. Second, it showed that nanotubes function well under biologically relevant conditions (salty water) and therefore offer great promise as biological sensors. The second accomplishment was the demonstration that a voltage pulse applied to an AFM tip could be used to electrically cut carbon nanotubes. We also showed that a carefully applied pulse could also 'nick' a nanotube, creating a tunnel barrier without completely breaking the tube. Nicking was employed to make, for example, a quantum dot within a nanotube.

McEuen, Paul L.↗
NASA NTRS2005

Multi-Scale Modeling of Cross-Linked Nanotube Materials

The effect of cross-linking single-walled carbon nanotubes on the Young's modulus of a nanotube-reinforced composite is modeled with a multi-scale method. The Young's modulus is predicted as a function of nanotube volume fraction and cross-link density. In this method, the constitutive properties of molecular representative volume elements are determined using molecular dynamics simulation and equivalent-continuum modeling. The Young's modulus is subsequently calculated for cross-linked nanotubes in a matrix which consists of the unreacted cross-linking agent. Two different cross-linking agents are used in this study, one that is short and rigid (Molecule A), and one that is long and flexible (Molecule B). Direct comparisons between the predicted elastic constants are made for the models in which the nanotubes are either covalently bonded or not chemically bonded to the cross-linking agent. At a nanotube volume fraction of 10%, the Young's modulus of Material A is not affected by nanotube crosslinking, while the Young's modulus of Material B is reduced by 64% when the nanotubes are cross-linked relative to the non-cross-linked material with the same matrix.

Frankland, S. J. V.↗
NASA NTRS2007

Process for making polymers comprising derivatized carbon nanotubes and compositions thereof

The present invention incorporates new processes for blending derivatized carbon nanotubes into polymer matrices to create new polymer/composite materials. When modified with suitable chemical groups using diazonium chemistry, the nanotubes can be made chemically compatible with a polymer matrix, allowing transfer of the properties of the nanotubes (such as mechanical strength) to the properties of the composite material as a whole. To achieve this, the derivatized (modified) carbon nanotubes are physically blended with the polymeric material, and/or, if desired, allowed to react at ambient or elevated temperature. These methods can be utilized to append functionalities to the nanotubes that will further covalently bond to the host polymer matrix, or directly between two tubes themselves. Furthermore, the nanotubes can be used as a generator of polymer growth, wherein the nanotubes are derivatized with a functional group that is an active part of a polymerization process, which would also result in a composite material in which the carbon nanotubes are chemically involved.

Tour, James M.↗
NASA NTRS2008

Process for separating metallic from semiconducting single-walled carbon nanotubes

A method for separating semiconducting single-walled carbon nanotubes from metallic single-walled carbon nanotubes is disclosed. The method utilizes separation agents that preferentially associate with semiconducting nanotubes due to the electrical nature of the nanotubes. The separation agents are those that have a planar orientation, .pi.-electrons available for association with the surface of the nanotubes, and also include a soluble portion of the molecule. Following preferential association of the separation agent with the semiconducting nanotubes, the agent/nanotubes complex is soluble and can be solubilized with the solution enriched in semiconducting nanotubes while the residual solid is enriched in metallic nanotubes.

Sun, Ya-Ping↗
NASA NTRS2009

Control of the Diameter and Chiral Angle Distributions during Production of Single-Wall Carbon Nanotubes

Many applications of single wall carbon nanotubes (SWCNT), especially in microelectronics, will benefit from use of certain (n,m) nanotube types (metallic, small gap semiconductor, etc.) Especially fascinating is the possibility of quantum conductors that require metallic armchair nanotubes. However, as produced SWCNT samples are polydisperse, with many (n,m) types present and typical approx.1:2 metal/semiconductor ratio. Nanotube nucleation models predict that armchair nuclei are energetically preferential due to formation of partial triple bonds along the armchair edge. However, nuclei can not reach any meaningful thermal equilibrium in a rapidly expanding and cooling plume of carbon clusters, leading to polydispersity. In the present work, SWCNTs were produced by a pulsed laser vaporization (PLV) technique. The carbon vapor plume cooling rate was either increased by change in the oven temperature (expansion into colder gas), or decreased via "warm-up" with a laser pulse at the moment of nucleation. The effect of oven temperature and "warm-up" on nanotube type population was studied via photoluminescence, UV-Vis-NIR absorption and Raman spectroscopy. It was found that reduced temperatures leads to smaller average diameters, progressively narrower diameter distributions, and some preference toward armchair structures. "Warm-up" shifts nanotube population towards arm-chair structures as well, but the effect is small. Possible improvement of the "warm-up" approach to produce armchair SWCNTs will be discussed. These results demonstrate that PLV production technique can provide at least partial control over the nanotube (n,m) population. In addition, these results have implications for the understanding the nanotube nucleation mechanism in the laser oven.

Nikolaev, Pavel↗
NASA NTRS2007

Carbon Nanotubes for Space Photovoltaic Applications

Carbon nanotubes (CNTs) can be envisioned as an individual graphene sheet rolled into a seamless cylinder (single-walled, SWNT), or concentric sheets as in the case of a multi-walled carbon nanotube (MWNT) (1). The role-up vector will determine the hexagonal arrangement and "chirality" of the graphene sheet, which will establish the nanotube to be metallic or semiconducting. The optoelectronic properties will depend directly on this chiral angle and the diameter of the SWNT, with semiconductor types exhibiting a band gap energy (2). Characteristic of MWNTs are the concentric graphene layers spaced 0.34 nm apart, with diameters from 10-200 nm and lengths up to hundreds of microns (2). In the case of SWNTs, the diameters range from 0.4 - 2 nm and lengths have been reported up to 1.5 cm (3). SWNTs have the distinguishable property of "bundling" together due to van der Waal's attractions to form "ropes." A comparison of these different structural types is shown in Figure 1. The use of SWNTS in space photovoltaic (PV) applications is attractive for a variety of reasons. Carbon nanotubes as a class of materials exhibit unprecedented optical, electrical, mechanical properties, with the added benefit of being nanoscale in size which fosters ideal interaction in nanomaterial-based devices like polymeric solar cells. The optical bandgap of semiconducting SWNTs can be varied from approx. 0.4 - 1.5 eV, with this property being inversely proportional to the nanotube diameter. Recent work at GE Global Research has shown where a single nanotube device can behave as an "ideal" pn diode (5). The SWNT was bridged over a SiO2 channel between Mo contacts and exhibited an ideality factor of 1, based on a fit of the current-voltage data using the diode equation. The measured PV efficiency under a 0.8 eV monochromatic illumination showed a power conversion efficiency of 0.2 %. However, the projected efficiency of these junctions is estimated to be > 5 %, especially when one considers the enhanced absorption (from nanotubes whose bandgap is tailored to illumination) and electromagnetic coupling in a network of nanotubes.

Efstathiadis, Harry↗
NASA NTRS2003

Carbon Nanotubes for Human Space Flight

Single-wall carbon nanotubes offer the promise of a new class of revolutionary materials for space applications. The Carbon Nanotube Project at NASA Johnson Space Center has been actively researching this new technology by investigating nanotube production methods (arc, laser, and HiPCO) and gaining a comprehensive understanding of raw and purified material using a wide range of characterization techniques. After production and purification, single wall carbon nanotubes are processed into composites for the enhancement of mechanical, electrical, and thermal properties. This "cradle-to-grave" approach to nanotube composites has given our team unique insights into the impact of post-production processing and dispersion on the resulting material properties. We are applying our experience and lessons-learned to developing new approaches toward nanotube material characterization, structural composite fabrication, and are also making advances in developing thermal management materials and electrically conductive materials in various polymer-nanotube systems. Some initial work has also been conducted with the goal of using carbon nanotubes in the creation of new ceramic materials for high temperature applications in thermal protection systems. Human space flight applications such as advanced life support and fuel cell technologies are also being investigated. This discussion will focus on the variety of applications under investigation.

Scott, Carl D.↗