Flame Synthesis of Single- and Multi-Walled Carbon Nanotubes and Nanofibers

Metal-catalyzed carbon nanotubes are highly sought for a diverse range of applications that include nanoelectronics, battery electrode material, catalysis, hydrogen storage media and reinforcing agents in polymer composites. These latter applications will require vast quantities of nanotubes at competitive prices to be economically feasible. Moreover, reinforcing applications may not require ultrahigh purity nanotubes. Indeed, functionalization of nanotubes to facilitate interfacial bonding within composites will naturally introduce defects into the tube walls, lessening their tensile strength. Current methods of aerosol synthesis of carbon nanotubes include laser ablation of composite targets of carbon and catalyst metal within high temperature furnaces and decomposition of a organometallics in hydrocarbons mixtures within a tube furnace. Common to each approach is the generation of particles in the presence of the reactive hydrocarbon species at elevated temperatures. In the laser-ablation approach, the situation is even more dynamic in that particles and nanotubes are borne during the transient cooling phase of the laser-induced plasma for which the temperature far exceeds that of the surrounding hot gases within the furnace process tube. A shared limitation is that more efficient methods of nanoparticle synthesis are not readily incorporated into these approaches. In contrast, combustion can quite naturally create nanomaterials such as carbon black. Flame synthesis is well known for its commercial scalability and energy efficiency. However, flames do present a complex chemical environment with steep gradients in temperature and species concentrations. Moreover, reaction times are limited within buoyant driven flows to tens of milliseconds. Therein microgravity can greatly lessen temperature and spatial gradients while allowing independent control of flame residence times. In preparation for defining the microgravity experiments, the work presented here focuses on the effect of catalyst particle size and reactant gas in 1g

Flame Synthesis Of Single-Walled Carbon Nanotubes And Nanofibers

Carbon nanotubes are widely sought for a variety of applications including gas storage, intercalation media, catalyst support and composite reinforcing material [1]. Each of these applications will require large scale quantities of CNTs. A second consideration is that some of these applications may require redispersal of the collected CNTs and attachment to a support structure. If the CNTs could be synthesized directly upon the support to be used in the end application, a tremendous savings in post-synthesis processing could be realized. Therein we have pursued both aerosol and supported catalyst synthesis of CNTs. Given space limitations, only the aerosol portion of the work is outlined here though results from both thrusts will be presented during the talk. Aerosol methods of SWNT, MWNT or nanofiber synthesis hold promise of large-scale production to supply the tonnage quantities these applications will require. Aerosol methods may potentially permit control of the catalyst particle size, offer continuous processing, provide highest product purity and most importantly, are scaleable. Only via economy of scale will the cost of CNTs be sufficient to realize the large-scale structural and power applications on both earth and in space. Present aerosol methods for SWNT synthesis include laser ablation of composite metalgraphite targets or thermal decomposition/pyrolysis of a sublimed or vaporized organometallic [2]. Both approaches, conducted within a high temperature furnace, have produced single-walled nanotubes (SWNTs). The former method requires sophisticated hardware and is inherently limited by the energy deposition that can be realized using pulsed laser light. The latter method, using expensive organometallics is difficult to control for SWNT synthesis given a range of gasparticle mixing conditions along variable temperature gradients; multi-walled nanotubes (MWNTs) are a far more likely end products. Both approaches require large energy expenditures and produce CNTs at prohibitive costs, around $500 per gram. Moreover these approaches do not possess demonstrated scalability. In contrast to these approaches, flame synthesis can be a very energy efficient, low-cost process [3]; a portion of the fuel serves as the heating source while the remainder serves as reactant. Moreover, flame systems are geometrically versatile as illustrated by innumerable boiler and furnace designs. Addressing scalability, flame systems are commercially used for producing megatonnage quantities of carbon black [4]. Although it presents a complex chemically reacting flow, a flame also offers many variables for control, e.g. temperature, chemical environment and residence times [5]. Despite these advantages, there are challenges to scaling flame synthesis as well

Laser-Induced Breakdown Spectroscopy of Trace Metals

An alternative approach for laser-induced breakdown spectroscopy (LIBS) determination of trace metal determination in liquids is demonstrated. The limits of detection (LOD) for the technique ranged from 10 ppb to 10 ppm for 15 metals metals (Mg, Al, Si, Ca, Ti, Cr, Fe, Co, Ni, Cu, Zn, As, Cd, Hg, Pb) tested

Single-Walled Carbon Nanotubes, Carbon Nanofibers and Laser-Induced Incandescence

Laser induced incandescence applied to a heterogeneous, multi-element reacting flows is characterized by a) temporally resolved emission spectra, time-resolved emission at selected detection wavelengths and fluence dependence. Laser fluences above 0.6 Joules per square centimeter at 1064 nm initiate laser-induced vaporization, yielding a lower incandescence intensity, as found through fluence dependence measurements. Spectrally derived temperatures show that values of excitation laser fluence beyond this value lead to a super-heated plasma, well above the vaporization of temperature of carbon. The temporal evolution of the emission signal at these fluences is consistent with plasma dissipation processes, not incandescence from solid-like structures

Laser Synthesis of Supported Catalysts for Carbon Nanotubes

Four methods of laser assisted catalyst generation for carbon nanotube (CNT) synthesis have been tested. These include pulsed laser transfer (PLT), photolytic deposition (PLD), photothermal deposition (PTD) and laser ablation deposition (LABD). Results from each method are compared based on CNT yield, morphology and structure. Under the conditions tested, the PLT was the easiest method to implement, required the least time and also yielded the best pattemation. The photolytic and photothermal methods required organometallics, extended processing time and partial vacuums. The latter two requirements also held for the ablation deposition approach. In addition to control of the substrate position, controlled deposition duration was necessary to achieve an active catalyst layer. Although all methods were tested on both metal and quartz substrates, only the quartz substrates proved to be inactive towards the deposited catalyst particles