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We have observed a nearly fourfold increase in the electron spin resonance (ESR) signal from an ensemble of single-walled carbon nanotubes (SWCNTs) due to oxygen desorption. By performing temperature-dependent ESR spectroscopy both before and after thermal annealing, we found that the ESR in SWCNTs can be reversibly altered via the molecular oxygen content in the samples. Independent of the presence of adsorbed oxygen, a Curie-law (spin susceptibility $\propto 1/T$) is seen from $\sim$4 K to 300 K, indicating that the probed spins are finite-level species. For both the pre-annealed and post-annealed sample conditions, the ESR linewidth decreased as the temperature was increased, a phenomenon we identify as motional narrowing. From the temperature dependence of the linewidth, we extracted an estimate of the intertube hopping frequency; for both sample conditions, we found this hopping frequency to be $\sim$100 GHz. Since the spin hopping frequency changes only slightly when oxygen is desorbed, we conclude that only the spin susceptibility, not spin transport, is affected by the presence of physisorbed molecular oxygen in SWCNT ensembles. Surprisingly, no linewidth change is observed when the amount of oxygen in the SWCNT sample is altered, contrary to other carbonaceous systems and certain 1D conducting polymers. We hypothesize that physisorbed molecular oxygen acts as an acceptor ($p$-type), compensating the donor-like ($n$-type) defects that are responsible for the ESR signal in bulk SWCNTs., Comment: 14 pages, 7 figures

The colors of suspended metallic colloidal particles are determined by their size-dependent plasma resonance, while those of semiconducting colloidal particles are determined by their size-dependent band gap. Here, we present a novel case for armchair carbon nanotubes, suspended in aqueous medium, for which the color depends on their size-dependent excitonic resonance, even though the individual particles are metallic. We observe distinct colors of a series of armchair-enriched nanotube suspensions, highlighting the unique coloration mechanism of these one-dimensional metals., Comment: 4 pages, 3 figures

We have measured temperature ($T$)- and power-dependent electron spin resonance in bulk single-wall carbon nanotubes to determine both the spin-lattice and spin-spin relaxation times, $T_1$ and $T_2$. We observe that $T_1^{-1}$ increases linearly with $T$ from 4 to 100 K, whereas $T_2^{-1}$ {\em decreases} by over a factor of two when $T$ is increased from 3 to 300 K. We interpret the $T_1^{-1} \propto T$ trend as spin-lattice relaxation via interaction with conduction electrons (Korringa law) and the decreasing $T$ dependence of $T_2^{-1}$ as motional narrowing. By analyzing the latter, we find the spin hopping frequency to be 285 GHz. Last, we show that the Dysonian lineshape asymmetry follows a three-dimensional variable-range hopping behavior from 3 to 20 K; from this scaling relation, we extract a localization length of the hopping spins to be $\sim$100 nm., Comment: 6 pages, 3 figures

Recent interest in developing new applications for carbon nanotubes (CNT) has fueled the need to use accurate macroscopic and nanoscopic techniques to characterize and understand their chemistry. X-ray photoelectron spectroscopy (XPS) has proved to be a useful analytical tool for nanoscale surface characterization of materials including carbon nanotubes. Recent nanotechnology research at NASA Johnson Space Center (NASA-JSC) helped to establish a characterization protocol for quality assessment for single wall carbon nanotubes (SWCNTs). Here, a review of some of the major factors of the XPS technique that can influence the quality of analytical data, suggestions for methods to maximize the quality of data obtained by XPS, and the development of a protocol for XPS characterization as a complementary technique for analyzing the purity and surface characteristics of SWCNTs is presented. The XPS protocol is then applied to a number of experiments including impurity analysis and the study of chemical modifications for SWCNTs.

This viewgraph presentation reviews the use of PICA (phenolic impregnated carbon ablator) as the selected material for heat shielding for future earth return vehicles. It briefly reviews the manufacturing of PICA and the advantages for the use of heat shielding, and then explains the reason for using Carbon Nanotubes to improve strength of phenolic resin that binds carbon fibers together. It reviews the work being done to create a carbon nanotube enhanced PICA. Also shown are various micrographic images of the various PICA materials.

Phenolic impregnated carbon ablator (PICA) is a thermal protection system (TPS) material developed at NASA Ames Research Center in the mid-90 s for Discovery missions. It was used on the Stardust return capsule heat shield which successfully executed the highest speed Earth entry to date on January 15, 2006. PICA is a porous fibrous carbon insulation infiltrated with phenolic resin, and is an excellent ablator that is effective for heating rates up to 1000 W/sq cm. It is one of several candidate TPS materials for the next generation of crewed spacecraft for Lunar and Mars missions. We will describe an ongoing research effort at NASA to improve mechanical properties of the phenolic matrix with carbon nanotubes. The aim is two-fold: to increase overall TPS strength during reentry and to improve Micrometeoroid/Orbital Debris (MMOD) protection in space. The former requires at least a good dispersion of nanotubes in phenolic, while the latter also requires covalent bonding between them to couple and transfer impact energy effectively from matrix to nanotubes. We will discuss the required chemical functionalization of nanotubes, processing issues and test results.

Electrochemical double-layer capacitors, or supercapacitors, have tremendous potential as high-power energy sources for use in low-weight hybrid systems for space exploration. Electrodes based on single-wall carbon nanotubes (SWCNTs) offer exceptional power and energy performance due to the high surface area, high conductivity, and the ability to functionalize the SWCNTs to optimize capacitor properties. This paper will report on the preparation of electrochemical capacitors incorporating SWCNT electrodes and their performance compared with existing commercial technology. Preliminary results indicate that substantial increases in power and energy density are possible. The effects of nanotube growth and processing methods on electrochemical capacitor performance is also presented. The compatibility of different SWCNTs and electrolytes was studied by varying the type of electrolyte ions that accumulate on the high-surface-area electrodes.

We explore Raman microprobe capabilities to visualize single wall carbon nanotubes (SWCNTs). Although this technique is limited to a micron scale, we demonstrate that images of individual SWCNTs, bundles or their agglomerates can be generated by mapping Raman active elementary excitations. We measured the Raman response from carbon vibrations in SWCNTs excited by confocal scanning of a focused laser beam. Carbon vibrations reveal key characteristics of SWCNTs as nanotube diameter distribution (radial breathing modes, RBM, 100-300 cm(exp -1)), presence of defects and functional groups (D-mode, 1300-1350 cm(exp -1)), strain and oxidation states of SWCNTs, as well as metallic or semiconducting character of the tubes encoded in the lineshape of the G-modes at 1520-1600 cm(exp - 1). In addition, SWCNTs are highly anisotropic scatterers. The Raman response from a SWCNT is maximal for incident light polarization parallel to the tube axis and vanishing for perpendicular directions. We show that the SWCNT bundle shape or direction can be determined, with some limitations, from a set of Raman images taken at two orthogonal directions of the incident light polarization.

The Raman spectra of singled-wall carbon nanotubes (SWNT) produced by laser and are process were studied between 5 and 500 kappa. The line width vs. temperature dependence of the low-frequency Raman bands between 150 and 200/ cm deviates from that expected for phonon decay through phonon-phonon scattering mechanism. The experimental results and their analysis provided convincing evidence that each of the low-frequency Raman lines is a superposition of several narrower Raman lines corresponding to tubes of nearly the same diameter. The application of Raman spectroscopy to probe the distribution of SWNT by both diameter and chirality is discussed.