EP1594821A4 - Process and apparatus for microwave desorption of elements or species from carbon nanotubes - Google Patents
Process and apparatus for microwave desorption of elements or species from carbon nanotubesInfo
- Publication number
- EP1594821A4 EP1594821A4 EP04704853A EP04704853A EP1594821A4 EP 1594821 A4 EP1594821 A4 EP 1594821A4 EP 04704853 A EP04704853 A EP 04704853A EP 04704853 A EP04704853 A EP 04704853A EP 1594821 A4 EP1594821 A4 EP 1594821A4
- Authority
- EP
- European Patent Office
- Prior art keywords
- microwave
- carbon nanotubes
- source
- hydrogen
- nanotubes
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/08—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor
- B01J19/12—Processes employing the direct application of electric or wave energy, or particle radiation; Apparatus therefor employing electromagnetic waves
- B01J19/122—Incoherent waves
- B01J19/126—Microwaves
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
- C01B3/0021—Carbon, e.g. active carbon, carbon nanotubes, fullerenes; Treatment thereof
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05B—ELECTRIC HEATING; ELECTRIC LIGHT SOURCES NOT OTHERWISE PROVIDED FOR; CIRCUIT ARRANGEMENTS FOR ELECTRIC LIGHT SOURCES, IN GENERAL
- H05B6/00—Heating by electric, magnetic or electromagnetic fields
- H05B6/64—Heating using microwaves
- H05B6/80—Apparatus for specific applications
- H05B6/806—Apparatus for specific applications for laboratory use
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/20—Nanotubes characterized by their properties
- C01B2202/26—Mechanical properties
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Definitions
- Hydride cells reduce the danger level of fuel cells which employ liquid hydrogen under pressure.
- these systems suffer from several disadvantages. They require a large amount of energy to desorb the hydrogen from the system. This high desorption energy reduces the overall efficiency of the engine. Fuel cell systems with these hydride cells while safe, may not see commercial use due to these two disadvantages. Hydride systems have seen production in a type of hybrid engine that employs a small fuel cell to power the automobiles engine at times of low energy consumption and an internal combustion engine during times of high power requirements.
- Carbon nanotubes fall into two major groups, multi-walled carbon nanotubes ("MWNTs”) and single-walled carbon nanotubes (“SWNTs"). There are a variety of techniques for fabricating SWNTs. Each of these fabrication techniques causes subtle yet important differences in the resulting nanotubes. These differences include changes in length and diameter, and as a
- Atty. Docket No. 122302.00013 2 result of these, the aspect ratio (defined as length/diameter).
- the aspect ratio can change by several orders of magnitude and alter the response of the nanotubes to electromagnetic waves.
- SWNTs are known to form into "ropes" or bundles.
- the first synthesis of carbon nanotubes was a by-product of the arc-discharge method in the fabrication of fullerenes. Their current methods of production are quite varied. These methods include arc-discharge, laser ablation, catalytic hydrocarbon decomposition and carbon monoxide disproportionation to carbon nanotubes plus carbon dioxide (HiPco Process).
- the MWNTs are made up of 2 to 50 concentric graphitic layers and have diameters in the range of 10 to 100 nanometers ("nm"). The SWNT is much thinner with diameters from 0.5 to 1.8 nm.
- MWNTs have high chemical stability and very high mechanical strength.
- the catalytic decomposition of hydrocarbons is a primary fabrication method of MWNTs.
- the MWNTs produced by this method are much purer than those obtained by the other methods with yields as high as 50% by weight of the deposits being MWNTs.
- the higher yields in turn require less purification, thus decreasing the cost of fabrication, as the majority of the material removed in the fabrication process is bulk carbon material.
- Critical aspects of production are length, diameter, and alignment, all of which can be controlled with this method of fabrication.
- SWNTs The structure of SWNTs is essentially rolled up graphite forming a very small, thin cylinder with no seam.
- the length and the diameter of these types of nanotubes are dependent on the type of metallic catalyst employed and the precise methodology used during fabrication.
- the maximum-recorded lengths have been in the cm length scale with diameters ranging from 0.5nm to 3nm.
- the structure and characteristics of SWNTs are closer to those of fullerenes than MWNTs.
- SWNTs are a novel one-dimensional material having many unique physical properties. MWNT properties are more closely approximated to bulk graphite.
- the catalysts typically used are Fe, Co, Ne, Cu, and Mg. In some experiments the catalysts have been combined in an effort to increase yields.
- SWNTs used in one embodiment of the present invention were produced via the HiPco (High Partial Pressure of CO) process.
- HiPco refers to a process of growing SWNTs using high pressure carbon monoxide in a vapor disproportionation process.
- nanotubes In order to be of any practical or commercial use, nanotubes must be produced with high levels of purity in large quantities.
- the HiPco process has shown some promise of being scaled up for large scale production and can also produce nanotubes that are > 90% pure.
- a reaction of Fe(CO) 5 and CO gas at high pressure and high temperature takes place.
- the metal catalyst atoms form larger clumps of material, approximately the size of the C 6 o molecule, they nucleate and form SWNTs. This occurs because a SWNT is a more stable form of carbon than what is in the chamber at this point in the process. Due to this, the carbon will preferentially take on the SWNT form.
- metal it is meant that there is a zero bandgap in the electronic structure or semi metallic with meVs of bandgap in semiconductor having about 1 meV of bandgap.
- the filling of the inner capillary of carbon nanotubes will contribute greatly to their use as fuel cell storage mediums. Presumably, this can be achieved through channeling of the hydrogen atom or molecule into the nanotube. If a beam of hydrogen atoms were incident on the walls of the nanotubes with energy levels of approximately 20eN, the atoms will rip through the wall and enter the nanotube. The defects in nanotubes on the scale caused by the channeling will self-repair in approximately 1 pico-second.
- the hydrogen atom may be placed inside the nanotubes by artificial implantation techniques.
- One of these methods is referred to as the "flip in” method. If the hydrogen atom is incident on the carbon nanotube with an energy of between 1.52eV and 20.0eN, the atom will react with the carbon on the exterior of the nanotubes and still have enough remaining energy to be 'flipped' to the interior of the nanotube. If less energetic hydrogen atoms are used, they will be repulsed, more energetic and the nanotube walls may be damaged according to one theory. There are still other theoretical methods of creating hydrogen rich nanotubes. These include the use of high-pressure, pure hydrogen environments and hydrogen environments provided during nanotube fabrication.
- Microwave radiation is a term used to describe a range of frequencies in the electromagnetic ("EM") spectrum typically in the range of 300 MHz to 300 GHz. These frequencies can be described in terms of wavelengths according to:
- This region contains a fairly wide range as compared to other portions of the EM spectrum. Due to the range of wavelengths, the region can be further subdivided into decimeter, centimeter, and millimeter waves.
- Microwaves existing at the lower end of the EM spectrum, when considering quantum energies, do not have sufficient energy to cause atoms to go from a ground state to an excited state. They are, in fact, several orders of magnitude away from being able to accomplish this directly. But they are able to couple to the transitions in the hyperfine structure of a dynamical state.
- the present invention has the advantage of, among other things, making fuel such as hydrogen or oxygen, or other gases, such as nitrogen or argon, available for use in a fraction of a second to a few seconds, rather than in minutes.
- the present invention comprises a process of applying a moderately powered microwave field (1.01 x 10 "5 eV) to SWNTs that contain an alternative fuel such as hydrogen or oxygen or other gas such as nitrogen or argon.
- the carbon nanotubes are heated as a result of their interaction with the microwaves.
- the technology used in generating microwaves is mature, such that microwave generators can be made portable with little difficulty. With adequate shielding, portable microwave sources can be made safe for use in vehicles or power generator applications.
- a microwave transparent container is used, advantageously, only the carbon nanotubes are heated.
- Conventionally available microwave transparent containers can be used in the process and apparatus of the present invention.
- Microwaves when properly applied to the carbon nanotubes, cause an absorbed or adsorbed gas, such as hydrogen or oxygen, or some other gaseous material, to escape the carbon nanotubes. The released gas can then be used for energy production.
- the carbon nanotubes useful for this process include SWNTs and multi-wall types. However, the use of carbon nanotubes with smaller aspect ratios is preferable as the hydrogen tends to bond better with highly damaged nanotubes. Undamaged carbon nanotubes also can be used advantageously in the present invention. Moreover, low
- Atty. Docket No. 122302.00013 10 wattage microwaves i.e. less than 100 W, can also be used to effectively heat nanotubes, thereby providing a safe level of power input and little to no degradative effect to the tube itself.
- Figure 1(a) illustrates SWNTs in an ultra high vacuum tube suspended above the microwave source wherein the tube is shown containing SWNTs under vacuum with room lights on and
- Figure 1(b) illustrates SWNTs under vacuum during microwave irradiation (2.45 GHz, 700 W) with the room lights off;
- Figures 2(a) and 2(b) illustrate the spectrum of light from raw and purified SWNTs when subjected to microwave irradiation
- Figure 3 is a plot of the spectra of light from both purified and unpurified HiPco Nanotubes as a microwave field is applied;
- Figure 4(a) is a schematic diagram of a two cavity klystron for generating microwaves
- Figure 4(b) is a schematic diagram of the reflex klyston for generating microwaves
- Figure 5(a) is the absorption spectrum of bucky paper in the range of 7 to 12 GHz;
- Figure 5(b) is an absorption spectrum of a 5 mg sample of purified SWNTs in the range of 7-12 GHz;
- Figure 5(c) is an absorption spectrum of a 5 mg sample of purified SWNTs in the range of 7-12 GHz of Figure 5(b), but with an expanded range in the y-axis;
- Figure 6 shows the results of desorption experiments from samples implanted with hydrogen and samples not implanted with hydrogen
- Figure 7 illustrates the TEM image of the fused carbon nanotubes after microwave irradiation
- Figure 8 illustrates TEM image showing looped carbon nanotubes after microwave irradiation
- Figure 9 is an RGA plot of outgassed materials from carbon nanotubes during microwave application.
- the process and apparatus of the present invention comprises subjecting carbon nanotubes containing a species, or elements such as hydrogen, oxygen, nitrogen and argon in air, in an inert gas chamber, in vacuum or under ultrahigh vacuum (“UHV”), to microwave radiation for certain predetermined amounts of time.
- a species, or elements such as hydrogen, oxygen, nitrogen and argon in air
- UHV ultrahigh vacuum
- the result of said process is heat release, light emission and gas evolution, accompanied by intense mechanical motion and carbon nanotube reconstruction; reconstruction only occurs if the microwave power is sufficiently high to result in heating of the nanotubes to greater than 1500°C.
- the apparatus of the present invention is any device that implements the described process.
- the present invention is improved over conventional methods with respect to, among other things, its efficiency and its safety characteristics. Further, the process and apparatus has the advantage of removing a gas, particularly hydrogen, much more quickly than any previous methods. Hydrogen can be removed from the carbon nanotubes on the order of seconds or fractions of a second, rather than minutes as is the case with conventional methods, h addition to removing hydrogen, the process of the present invention removes other gases that may be used as fuel sources from carbon nanotubes, such as oxygen. In one embodiment of the present invention, the amount of hydrogen removed from the carbon nanotubes is shown to be approximately 100
- SWNTs used in one embodiment of the present invention were produced via the HiPco (High Partial Pressure of CO) process.
- HiPco refers to a process of growing SWNTs using high pressure carbon monoxide in a vapor disproportionation process.
- nanotubes must be produced with high levels of purity in large quantities.
- the HiPco process has shown some promise of being scaled up for large scale production and can also produce nanotubes that are > 90%> pure.
- a reaction of Fe(CO) 5 and CO gas at high pressure and high temperature takes place. When the metal catalyst atoms form larger clumps of material, approximately the size of the C 6 o molecule, they nucleate and form SWNTs.
- HiPco nanotubes display strong microwave absorption characteristics, e.g., 1.01 x 10 "5 eN microwave field, with subsequent light emission, intense heat release, outgassing, mechanical extension and nanotube reconstruction. SWNTs produced via other processes can also be used in the process and apparatus of the present invention.
- SWNTs hi air and under application of the microwave field, SWNTs ignite and burn.
- the regions of the SWNTs that undergo this process show a permanent color change from black to orange. These orange regions fluoresce under normal room light.
- a TEM image of these orange regions shows a change to amorphous carbon structures that are 50-500 nm in diameter with no discernable tube structure.
- the purified nanotubes when in the presence of the microwave field in air, only display random scintillation of white light.
- a novel reaction occurs when either purified or raw SWNTs are exposed to microwaves under conditions of vacuum of approximately between 10 "4 torr and 10 "8 torr pursuant to one embodiment of the present invention.
- the microwave frequency can be between 0.1 GHz and 100 GHz, including in one embodiment about 2.45 GHz, and the microwave power between 0.1 Watt and 1,500 Watts or where the microwave field incident on the carbon nanotubes is about 1.01 x 10 "5 eN.
- Carbon nanotubes in the vacuum system caused higher levels of vacuum (lower pressures) to be reached than normally observed, possibly due to molecular gas adsorption by the carbon nanotubes.
- FIG. 9 is a plot 900 of the residual gas analysis ("RGA") of outgassed atomic masses from pure HiPco nanotubes during microwave field application.
- the spike at located at atomic mass unit 2 represents hydrogen in molecular form. This chart is in a log scale and the quantity of hydrogen removed is approximately 100 times more than any other atomic mass. Short exposure pulses of approximately 3 to 5 seconds can be repeated with no obvious degradation over the 35 pulses attempted.
- Figure 1(a) illustrates SWNTs 100 in an ultra high vacuum tube 101 suspended above the microwave source wherein the tube is shown containing SWNTs under vacuum with room lights on.
- Figure 1(a) shows a sample of HiPco nanotubes as a microwave field is applied.
- Figure 1(b) illustrates SWNTs 100 in an ultra high vacuum tube 101 suspended above the microwave source wherein the tube is shown containing SWNTs under vacuum
- the light emission under UHN conditions is accompanied by outgassing in both the crude and purified carbon nanotubes.
- the expelled gas is what was previously adsorbed by the carbon nanotubes and consists primarily of hydrogen, as observed using a residual gas analyzer ("RGA").
- RAA residual gas analyzer
- the described embodiment of the present invention shows microwave fields to be an efficient method for extracting hydrogen from carbon nanotubes. The emission of light from the carbon nanotubes continues after the hydrogen is desorbed.
- the microwave irradiation of the samples in the described embodiment of the present invention is accompanied by a very rapid temperature increase in the samples.
- Figure 3 is a plot 300 of the spectra of light from both purified and unpurified HiPco nanotubes as microwave field is applied.
- the wavelength is in nanometers and the intensity is in arbitrary units. It should be noticed that most of the peaks are in the same locations on both samples, merely showing different intensities.
- One embodiment of the present invention utilizes a microwave source comprising a 700 watt magnetron at 2.45 GHz located proximate to the SWNTs, such that microwave radiation is incident upon the SWNT.
- Other microwave sources at different power and frequency settings can also be utilized.
- SWNTs were tested in both the purified and raw conditions. It is often necessary to generate a microwave signal. The generation of low frequency EM signals is usually achieved via the transfer of electrical energy from a steady electric field into an alternating field. In this situation, a signal with the desired frequency is always present. This is typically due to thermal noise. The desired frequency is then selectively amplified to the desired power level by feedback with the phase relation that is appropriate to the application. This technique works reasonably well for frequencies up to approximately 1 GHz.
- Atty. Docket No. 122302.00013 16 have a degrading effect on such things as the oscillator circuit, rendering signal sources very poor without a change of the generation technique.
- a specially designed dual cavity klystron 400 with planar triodes is typically employed for signal sources in these ranges.
- the electron transit time has no effect on these devices due to their geometry.
- These devices consist of small distances between the triodes and a high accelerating voltage.
- These triodes are used in conjunction with a tunable dual-resonant cavity. These devices can typically be retimed to a significant portion of the 1 to 10 GHz portion of the microwave spectrum, and the maximum power output from such a device is in the range of 10 Watts.
- these dual cavity klystrons consist of two resonant cavities in tandem through which passes an electron beam.
- a radio frequency (“RF") field in the first of the two cavities, will bunch the electrons into groups. These groups then pass into the second cavity and induce an RF field.
- the first of the two cavities slightly accelerates some electrons, while others are slowed down.
- the acceleration and deceleration is determined by which portion of the RF cycle the electrons are in. After several millimeters of transit, the faster electrons will catch the slower ones and the maximum allowable "bunching" will occur. It is at exactly this position that the second of the two resonant cavities is situated. Further along the beam line the accelerated electrons have passed the slower ones and the electrons are again debunched.
- the klystron will become an oscillator.
- the frequency of oscillation is determined by the resonant frequencies of the cavities (which can be adjusted by changing their physical size).
- the accelerator voltage may cause a small change in the oscillation frequency.
- reflex klystron 401 is simplified over the dual cavity version by removal of one of the two cavities.
- BWO Backward wave oscillators
- a much higher power level is required from a microwave source.
- These applications typically employ a magnetron.
- a static magnetic field is applied perpendicularly to the electron beam. This is to force the electrons into a nearly circular path. This will extend the amount of interaction time and allow a much higher power level to be achieved.
- Atty. Docket No. 122302.00013 18 line techniques are employed to reduce the physical size of the circuits. These sources are quite versatile, offering excellent frequency stability, on the order of one part in 10 9 , over a wide range of frequencies. These sources are typically very low power, on the order of lOOmW.
- the local oscillator frequency must cause the IF to equal the frequency of an IF filter.
- the filter device allows the signal to be amplified over only a small bandwidth by amplifiers. By using this principle, the frequency of the detected signal is transformed to a lower frequency (between 10MHz and 300MHz typically). It is in this lower range that amplifiers produce far less noise. This type of receiver tends to have a much improved signal-to-noise ratio, making it superior to diodes by a factor as large as 10 5 .
- twin channel superheterodyne receivers are employed.
- the second channel can be employed to lock the signal frequency by an automatic frequency control unit. This allows for signal sources which do not 'drift'. Many newer systems will frequently use a network analyzer, hi these systems a swept, or stepped frequency source, is locked into a
- Atty. Docket No. 122302.00013 19 superheterodyne receiver Vector network analyzers use a dual channel receiver to measure ratios of amplitudes and the differences in phase for the two signals fed in. It is, therefore, capable of determining the real and imaginary parts of an unknown 2 port device. These analyzers typically come packaged with a computer to allow automated measurements, suitable processing of signals such as signal averaging and filtering of background noise. These types of computer controlled devices are intended to reduce errors. The system will attempt to remove what it determines to be systematic errors and display what it thinks is the correct measurement, based on a statistical analysis algorithm, which in many cases tends to remove important details.
- Waveguides are basically hollow pipes and are available in many different geometries. Most common are the rectangular and circular waveguides. There are two types of field configurations inside waveguides. The first has the electric field component in the direction of the wave propagation (TM-modes) and the second has the magnetic field in the direction of wave propagation (TE-modes). For certain configurations, which are dependent on the
- Waveguides Atty. Docket No. 122302.00013 20 frequency range used, various physical sizes of waveguides are necessary. This change in size is due to the changes in wavelength associated with the shift in the frequency being examined. Waveguides also do not suffer from the sometimes an enormous amount of signal degradation and loss that can occur in wires making them a far superior method of signal transmission.
- Buckypaper is a thin membrane of purified SWNTs. There is generally no alignment of the tubes in buckypaper and the thickness of the membrane depends on the sample preparation protocol, but it is generally 1-100 microns thick.
- absorption spectra of buckypaper over the range of 7 to 12 GHz can be seen. This spectrum was taken with a sweep source and consists of 25 sweeps across the entire range. The results shown are the average of these sweeps to remove experimental error sources. The signals recorded are the transmitted and reflected power levels, which were then added together, and subtracted from the reference voltage. The original reference voltage was then divided into this voltage in order to obtain the "percent" of the microwave signal absorbed by the bucky paper.
- Carbon nanotubes are known, according to the published work of the inventors, to be efficient microwave absorbers. Normally, long chain molecules absorb over a wide range of frequencies. A group of nanotubes, such as that found in buckypaper, is essentially a large group of very long-chain molecules. These molecules will have different length distributions and the microwaves and nanotubes interact in different ways based on the distribution of lengths.
- Figure 5(b) and 5(c) an absorption spectrum in the range of 7 to 12 GHz of 5 mg of purified SWNTs can be seen. This shows a larger absorption, which is to be expected, with the increased number of long chain molecules in the sample. These broad-extended, range interactions are not only unusual but, appear to be very useful.
- A is the largest rotational constant of an asymmetric rotor.
- L Electronic angular momentum of an entire atom or molecule
- S Electron Spin Angular Momentum.
- Another mechanism might involve a microwave interaction with iron nanoparticles that occupy the end of the nanotubes. Upon irradiation with microwaves, the iron nanoparticles efficiently absorbs the microwave and transmits the energy to the nanotube to which it is coupled.
- a third mechanism could involve an excitation of nanotube electrons from one or more of the tube types (i.e., the semi metallic tubes) into an electron plasma that coats the tube surface. This would account for the light emission and the apparent material expansion during the irradiation cycles.
- the microwave sources are very low power sources, which is typical when performing spectroscopic measurements.
- nanotubes In order to be of commercial interest in many cases, nanotubes must be able to interact efficiently with high power microwave signals, hi the embodiment of the present invention, operating at 2.45 GHz with 750Wats of power can be employed.
- Atty. Docket No. 122302.00013 23 normal background were observed from purified SWNTs where average diameters near 1 nm. This radiation may indicate emissions in the soft x-ray region.
- the temperatures of both physical and raw SWNTs of the system were observed using a pyrometer that measures blackbody radiation at 2 ⁇ m. These observed temperatures were in the range of 2000° C.
- SWNTs are mechanically extremely supple, with a wide range of motions possible without destroying the integrity of the nanotubes.
- the build-up of the phonon spectrum, since its origin is the dynamical motion of nanotubes, will take seconds. This time scale corresponds to the delay seen before visible radiation occurs.
- the phonon frequency will match the absorption frequency of the outer electrons in the nanotube structure, and they will be ionized, although not intending to be bound by any particular mechanism.
- This process forms an electron plasma which exchanges energy with the phonon sea.
- the electron plasma Once the electron plasma reaches the plasma edge, it will radiate in the optical, UN and soft X-ray regions, absorbing and reradiating most of the incident energy in a steady state equilibrium. The entire sample seems to radiate as a single object, due to electron coupling among the nanotubes, which form a "giant dipole resonator.” This system can both absorb and emit electromagnetic energy very efficiently.
- SW ⁇ Ts that have a diameter of one nanometer make them quantum waveguides that delocalize electrons in their interior, adding to the effect by increasing the effective collision cross section.
- a single nanotube
- Atty. Docket No. 122302.00013 24 which is immersed in such a dense spectrum of phonon states, can be considered as a single extended quasi-particle. To a first approximation, it can be thought of as a physical realization of a one-dimensional quantum string.
- the coupling among nanotubes is so strong, due to phonon and electron exchange, that the material has collective dynamics.
- Visual reactions to the application of the microwaves to the HiPco SWNTs took place approximately 1 second after application of the microwave field.
- Laser-oven-generated SWNTs were also utilized. The reactions from this type of SWNT were not easily observable, due, perhaps, to the increased average diameters in these types of SWNTs vs. the HiPco SWNTs or differing amounts of iron remaining in the sample.
- Another aspect of the present invention comprises a process and apparatus for filling of the inner capillary of nanotubes with hydrogen.
- a beam of hydrogen atoms were incident on the walls of the nanotubes with energy levels of approximately 20eV they will rip through the wall and enter the nanotube. The defects caused in nanotubes on the scale of which would be caused by the channeling will self-repair in approximately 1 picosecond.
- An accelerator was used to implement the ion beam line process. The energy of an accelerated beam of hydrogen. To implement the channeling process, a 4 mg sample was run in the ion beam line with the incident energy of hydrogen impact the carbon nanotubes of 5 keV.
- the hydrogen slows down as it passes through more and more nanotubes until it is finally captured the implantation.
- the particle rate was approximately 1 particle every 10 "9 seconds which is slow enough to allow the self-repairing of the nanotubes.
- the sample was placed in the apparatus in such a way to measure not only the total charge incident on the sample but also what charge channeled through. This allowed the total number of trapped particles to be determined to be approximately 10 17 hydrogen atoms.
- a first sample consisted of 4 mg of Atty. Docket No. 122302.00013 25 SWNTs which had not been implanted with hydrogen via the beam line implantation method, but were bathed in an environment of approximately 100 torr of hydrogen for 1 hour.
- a second sample was also bathed in an environment of 100 torr of hydrogen for 1 hour and then implanted with approximately 10 17 hydrogen atoms.
- the results 600 of the subsequent desorption experiment show a large increase in the amount of stored hydrogen.
- the levels of hydrogen in the vacuum system rose from about 10 "9 torr to about 10 "5 torr.
- FIG. 9 is an RGA plot 900 of outgassed materials from carbon nanotubes during microwave application.
- Another aspect of the present invention is as an effective means of welding nanotubes or nanotube-based ropes in their pure states or after dispersion in blends or composites, thereby altering the mechanical properties of the final materials.
- TEM imaging of the carbon nanotubes after microwave irradiation in UHV showed that many of the nanotubes fused or welded into neighboring tubes to form junctions.
- the well-defined junction formations 700 can be seen in Figure 7.
- looped structures 800 formed and are abundant in the irradiated tubes.
- the welding of SWNTs requires breaking of carbon bonds and rearrangement of the carbon atoms. In order for this to take place, temperatures must reach at least 1500°C, indicative of an efficient absorption of microwaves. It is well known that frequency up- conversion occurs in these regions in pyroelectric crystals. A similar mechanism may be at work in the SWNTs.
- the process and apparatus of the present invention described herein is an effective means of welding nanotubes or
- SWNTs When exposed to microwave fields SWNTs show intense broadband light emission, extreme heating, outgassing of previously adsorbed materials, and tube reconstruction. As noted, the expulsion of hydrogen from the carbon nanotubes is adaptable in a plurality of applications, including in reusable fuel cells.
- the present invention can be particularly adapted for use in fuel cell storage in vehicles, including automobiles and small disposable fuel cell sources for rocketry, and gas fuel storage for long term space missions. Advantages of this process and apparatus are cost effectiveness, safety and recyclable fuel cell material. Further, the field emissions in the UN region, with the peak intensity at approximately 328 nm, which corresponds to a known carbon emission line, may find application as a UN laser source.
- Some of the hydrogen may be inside of the nanotubes, thereby becoming ionized and forming a plasma, which would contribute to the UV-emission being observed.
- the mechanical explanation of the out-gassing of the hydrogen in the present invention is due to tube flexure as well as phonon collision resulting from high temperatures. Additional applications of the process of the present invention include portable heating sources for many uses, including military use, and as small, portable, high yield power battery sources.
- the present invention includes both the process described herein and any apparatus that is constructed to implement the process described herein.
Abstract
Description
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US20050118092A1 (en) * | 2003-09-29 | 2005-06-02 | David Allara | Apparatus and method for inducing electrical property changes in carbon nanotubes |
US7611687B1 (en) * | 2004-11-17 | 2009-11-03 | Honda Motor Co., Ltd. | Welding of carbon single-walled nanotubes by microwave treatment |
JP2007186353A (en) * | 2006-01-11 | 2007-07-26 | Mie Univ | Method for treating surface adherence of carbon nanotube |
US8257472B2 (en) | 2008-08-07 | 2012-09-04 | Raytheon Company | Fuel removal system for hydrogen implanted in a nanostructure material |
CN101966446A (en) * | 2010-09-02 | 2011-02-09 | 安徽农业大学 | Method for preparing absorption-photocatalysis double-function coupling material by utilizing agricultural wastes |
CN107029645A (en) * | 2017-05-12 | 2017-08-11 | 武汉喜玛拉雅光电科技股份有限公司 | A kind of continuous microwave synthesizer and the method that platinum carbon catalyst is prepared with it |
CN111065178A (en) * | 2020-01-17 | 2020-04-24 | 湖南三重理想储能科技有限公司 | Microwave heating device for energy storage medium and adsorption medium |
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WO2003040446A2 (en) * | 2001-06-15 | 2003-05-15 | The Pennsylvania State Research Foundation | Method of purifying nanotubes and nanofibers using electromagnetic radiation |
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DE2934607A1 (en) * | 1979-08-28 | 1981-03-12 | Huther & Co, 6521 Bechtheim | Drying system for flammable loose material - has conveyor carrying material through oven using microwaves to dry material and has vacuum system |
US6420457B1 (en) * | 2000-04-04 | 2002-07-16 | Westinghouse Savannah River Company, Llc | Microwave treatment of vulcanized rubber |
KR20020046342A (en) * | 2000-12-12 | 2002-06-21 | 엘지전자 주식회사 | Part heating apparatus using a carbon nanotube and application method thereof |
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