A purification method has been developed that provides for the removal of metal catalysts and impurity carbon from laser-oven-grown single-wall carbon nanotube (SWNT) material. The oxidation rate of SWNTs in air at elevated temperatures is correlated to the metal content of the sample. Sample purity is documented with SEM, TEM, electron microprobe analysis, Raman, and UV-vis-near-IR. We also note that the relative intensity of the electronic transitions in the near-infrared to the continuum absorption at 400 nm in the UV serves as a useful monitor of the perturbation of the sidewall π-electron density of SWNTs due to sidewall substitution and/or oxidation.

A purification method has been developed that provides for the removal of metal catalysts and impurity carbon from laser-oven-grown single-wall carbon nanotube (SWNT) material. The oxidation rate of SWNTs in air at elevated temperatures is correlated to the metal content of the sample. Sample purity is documented with SEM, TEM, electron microprobe analysis, Raman, and UV-vis-near-IR. We also note that the relative intensity of the electronic transitions in the near-infrared to the continuum absorption at 400 nm in the UV serves as a useful monitor of the perturbation of the sidewall π-electron density of SWNTs due to sidewall substitution and/or oxidation.

The growth of a continuous, uniform Au layer on a dielectric nanoparticle is the critical step in the synthesis of nanoparticles such as nanoshells or nanorice, giving rise to their unique geometry-dependent plasmon resonant properties. Here we report a novel, streamlined method for Au layer metallization on prepared nanoparticle surfaces using carbon monoxide as the reducing agent. This approach consistently yields plasmonic nanoparticles with highly regular shell layers and is immune to variations in precursor or reagent preparation. Single particle spectroscopy combined with scanning electron microscopy reveal that thinner, more uniform shell layers with correspondingly redshifted optical resonances are achievable with this approach.

Mass spectrometry imaging (MSI) of tissue implanted with silver nanoparticulate (AgNP) matrix generates reproducible imaging of lipids in rodent models of disease and injury. Gas-phase production and acceleration of size-selected 8 nm AgNP is followed by controlled ion beam rastering and soft landing implantation of 500 eV AgNP into tissue. Focused 337 nm laser desorption produces high quality images for most lipid classes in rat brain tissue (in positive mode: galactoceramides, diacylglycerols, ceramides, phosphatidylcholines, cholesteryl ester, and cholesterol, and in negative ion mode: phosphatidylethanolamides, sulfatides, phosphatidylinositol, and sphingomyelins). Image reproducibility in serial sections of brain tissue is achieved within <10% tolerance by selecting argentated instead of alkali cationized ions. The imaging of brain tissues spotted with pure standards was used to demonstrate that Ag cationized ceramide and diacylglycerol ions are from intact, endogenous species. In contrast, almost all Ag cationized fatty acid ions are a result of fragmentations of numerous lipid types having the fatty acid as a subunit. Almost no argentated intact fatty acid ions come from the pure fatty acid standard on tissue. Graphical Abstract ᅟ.

Survey studies of pressure−temperature-induced transformations of single-wall carbon nanotubes (SWNT) at 1.5, 8.0, and 9.5 GPa and temperatures ranging from 200 to 1500 °C in a piston-cylinder or “Toroid” type high pressure devices have been carried out. It was found that the combined effects of high pressures and high temperatures produce irreversible changes in the SWNT structure, in contrast with the reversible effect of high pressure alone, previously studied by several research groups. The Raman, electron microscopy, and X-ray diffraction data obtained in the present work provide evidence for covalent interlinking of SWNT by sp3 C−C bonds which escalates with the increasing treatment temperature and pressure. The formation of new carbon structures such as nano- and microcrystalline diamond-like (cubic and hexagonal) and nanographite phases under higher pressures (8.0 and 9.5 GPa) has been observed.

Large fullerenes and carbon-coated metal nanoparticles that are formed during the synthesis of carbon nanotubes have been functionalized by the addition of alkyl radicals and isolated by extraction into chloroform. The soluble, functionalized fullerenes have been isolated from raw single-wall carbon nanotube (SWNT) material prepared by laser oven, direct current arc, and high-pressure carbon monoxide production methods. Analyses of the extracted large fullerenes were carried out by thermogravimetric analysis, UV-vis-near-IR, laser desorption ionization mass spectrometry, and high-resolution transmission electron microscopy.

The Billups-Birch Reduction chemistry has been shown to functionalize single-walled carbon nanotubes (SWCNTs) without damaging the sidewalls, but has challenges in scalability. Currently published work uses a large mole ratio of Li to carbon atoms in the SWCNT (Li:C) to account for lithium amide formation, however this increases the cost and hazard of the reaction. We report here the systematic understanding of the effect of various parameters on the extent of functionalization using resonant Raman spectroscopy. Addition of 1-iodododecane yielded alkyl-functionalized SWCNTs, which were isolated by solvent extraction and evaporation, and purified by a hydrocarbon wash. The presence of SWCNT growth catalyst residue (Fe) was shown to have a strong adverse effect on SWCNT functionalization. Chlorination-based SWCNT purification reduced the amount of residual Fe, and achieve a maximum I/I ratio using a Li:C ratio of 6:1 in a reaction time of 30 min. This result is consistent with published literature requiring 20-fold mole equivalents of Li per mole SWCNT with a reaction time of over 12 h. This new understanding of the factors influencing the functionalization chemistry will help cut down material and process costs, and also increase the selectivity of the reaction toward the desired product.

The nonselective nature of glucose pyrolysis chemistry can be controlled by preventing the sugar ring from opening and fragmenting.