U.S. patent application number 12/770704 was filed with the patent office on 2010-11-04 for systems, devices, and/or methods regarding specific precursors or tube control agent for the synthesis of carbon nanofiber and nanotube.
This patent application is currently assigned to TH LLC. Invention is credited to Nguyen Khe.
Application Number | 20100278715 12/770704 |
Document ID | / |
Family ID | 43030489 |
Filed Date | 2010-11-04 |
United States Patent
Application |
20100278715 |
Kind Code |
A1 |
Khe; Nguyen |
November 4, 2010 |
Systems, Devices, and/or Methods Regarding Specific Precursors or
Tube Control Agent for the Synthesis of Carbon Nanofiber and
Nanotube
Abstract
Certain exemplary embodiments can comprise, via a tube control
agent (TCA) and a metallic catalyst, producing a carbon nanotube.
At least some carbon used to form the carbon nanotube can be
obtained from a plant, a cellulose product, and/or a cellulosic
product. At least some of the carbon can be converted into
powder.
Inventors: |
Khe; Nguyen; (Ho Chi Minh
City, VN) |
Correspondence
Address: |
Zobrist Law Group
3 Boar's Head Lane
Charlottesville
VA
22903
US
|
Assignee: |
TH LLC
Hanoi
VN
|
Family ID: |
43030489 |
Appl. No.: |
12/770704 |
Filed: |
April 29, 2010 |
Related U.S. Patent Documents
|
|
|
|
|
|
Application
Number |
Filing Date |
Patent Number |
|
|
61173777 |
Apr 29, 2009 |
|
|
|
Current U.S.
Class: |
423/447.1 ;
977/742 |
Current CPC
Class: |
B82Y 40/00 20130101;
H01G 11/36 20130101; D01F 9/127 20130101; Y02E 60/13 20130101; C01B
32/15 20170801; B82Y 30/00 20130101 |
Class at
Publication: |
423/447.1 ;
977/742 |
International
Class: |
D01F 9/12 20060101
D01F009/12 |
Claims
1. A method comprising a plurality of activities, comprising: via a
carbon nanotube, a carbon nano fiber, or functionalized nano carbon
fabricating an item comprising: components adapted for use as armor
or a covering that at least partially resists penetration by a
projectile, radiation, chemical agents, or biological agents; thin
film prepared by the solvent evaporation of the foregoing adhesive
surfaces; apparel, footwear, or fabrics adapted for use as a tarp,
weather-resistant covering, or sail; substrates adapted for
acoustic, infrared, ultraviolet, or other electromagnetic radiation
detection; substrates adapted to form tires, railroad bogies,
friction control, or vibration control devices; load-bearing lines
adapted for use in parachutes, draglines, cargo containers,
netting, or connecting lines; moorings adapted for land-based,
aquatic, aerial, or outer space applications; structures adapted
for load-bearing or retention applications in construction,
including buildings, scaffolds, marine vessel hulls, components, or
fittings; construction materials adapted for use in structures;
metallic alloys adapted for use in structures, said metallic alloys
comprising nano carbon structures and at least one metal; ceramic
composites adapted for use in structures, said ceramic composites
comprising nano carbon structures and at least one ceramic
material; a structure comprising a heat resistant composite adapted
to resist thermal decomposition to at least 1500 degrees Celsius;
superconductor composites adapted for use in structures, said
superconductor composites prepared at temperature higher than 1500
degrees Celsius, said superconductor composites comprising nano
carbon structures and at least one superconducting material; high
temperature composites adapted for use in structures; aircraft or
aerospace fuselages or structures, or land-based vehicle
components, including body parts, engine components, or brake
linings; rotation parts adapted for use in at least one of:
vehicles; transportation devices, rotating equipment; or rotating
tools; bearings; composites adapted for use in paints adapted to
resist scratches and wear caused by an impact or collision;
colorants adapted for use in ceramic coloration process, processing
at high heat condition; composites adapted for use in brick;
composites adapted for use in biomechanical devices; surgical
implants; tissue-engineering structures including bone, tendon,
muscle, nerve, skin implants or surrogates; wound-healing
structures, or molecular capture devices adapted for timed drug
delivery; nano-cantilevers adapted for biosensing, cell growth, or
orthopedic, vascular, or neural prostheses; filters, barriers, or
wipes; sheets, substrates, nanowires, ultrathin films, or photon
detectors adapted for conducting electricity or acting as
batteries, membrane fuel cells, supercapacitors, superconductors,
electromagnetic or electro-optical actuators, or
microelectromechanical devices; sheets or structures with variable
optical properties; sheets adapted for use as heat conductors, heat
sinks, building and reinforcing material, automotive, marine, or
aviation or aerospace panels; tubular or I-beam cross sectional
items adapted for use as conduits or structural members; or an
electron source adapted for use in: electron microscopy; field
emission lighting; x-ray source; space propulsion; traveling wave
tube amplifiers; air remediation; water remediation; or cold field
emission; said carbon nanotube produced via a tube control agent
(TCA) and a metallic catalyst, at least some carbon used to form
said carbon nanotube obtained from starch, a bean bearing plant,
cloth, wood, a plant, cellulose or a cellulosic product; said at
least some carbon converted into powder by at least one of:
mechanical milling, biochemical reaction, and chemical
reaction.
2. The method of claim 1, further comprising: via a process
utilizing said TCA and said metal catalyst, controlling a length
and diameter of said, carbon nanotube, said carbon nano fiber, or
said functionalized nano carbon.
3. The method of claim 1, wherein: said at least some carbon used
to form said carbon nanotube is obtained from starch.
4. The method of claim 1, wherein: said at least some carbon used
to form said carbon nanotube is obtained from said bean bearing
plant.
5. The method of claim 1, wherein: said at least some carbon used
to form said carbon nanotube is obtained from cloth.
6. The method of claim 1, wherein: said at least some carbon used
to form said carbon nanotube is obtained from wood.
7. The method of claim 1, wherein: said at least some carbon used
to form said carbon nanotube is obtained from said plant.
8. The method of claim 1, wherein: said at least some carbon used
to form said carbon nanotube is obtained from cellulose.
9. The method of claim 1, wherein: said at least some carbon used
to form said carbon nanotube is obtained from said cellulosic
product.
10. The method of claim 1, wherein: said TCA comprises a unit
having a structure formula: ##STR00023## in which each of R.sub.1,
R.sub.2, and R.sub.3 is selected from hydrogen, alkyl, alkoxy,
alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or without hetero
atoms, with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.4R.sub.5, --NR.sub.6H, --NH.sub.2,
--COOH, --CO, --COOR.sub.S, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.8R.sub.9, or--COCl.
11. The method of claim 1, wherein: said TCA comprises a unit
having a structure formula: ##STR00024## in which each of R.sub.1
and R.sub.2 is selected from hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.3R.sub.4, --NR.sub.5H, --NH.sub.2,
--COOH, --CO, --COOR.sub.6, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.7R.sub.8, or --COCl.
12. The method of claim 1, wherein: said TCA comprises a unit
having a structure formula: ##STR00025## in which R.sub.1 is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.2R.sub.3, --NR.sub.4H, --NH.sub.2, --COOH, --CO,
--COOR.sub.5, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.6R.sub.7, or
--COCl.
13. The method of claim 1, wherein: said TCA comprises a unit
having a structure formula: ##STR00026## in which said formula
comprises a 3 member ring, 4 member ring, 5 member ring, 6 member
ring, 7 member ring, or 8 member ring having substituent groups
including hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, or aryl, with or without hetero atoms, with or
without substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.1R.sub.2, --NR.sub.3H, --NH.sub.2, --COOH, --CO,
--COOR.sub.4, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.5R.sub.6,
--COCl, wherein member rings are saturated and unsaturated with a
value of n between 1 and 6; said member rings comprising benzene,
napthalene, anthracene, perylene, or perinone.
14. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00027## in which each of
R.sub.1, R.sub.2, and R.sub.3 is selected from hydrogen, alkyl,
alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5, --NR.sub.6H,
--NH.sub.2, --COOH, --CO, --COOR.sub.S, --O--, --CHO, --S--,
--SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl.
15. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00028## in which R is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.2R.sub.3, --NR.sub.4H, --NH.sub.2, --COOH, --CO,
--COOR.sub.5, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.6R.sub.7, or
--COCl.
16. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00029## in which each of
R.sub.1 and R.sub.2 is selected from hydrogen, alkyl, alkoxy,
alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or without hetero
atoms, with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.3R.sub.4, --NR.sub.5H, --NH.sub.2,
--COOH, --CO, --COOR.sub.6, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.7R.sub.8, or --COCl.
17. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00030## in which each of
R.sub.1, R.sub.2, and R.sub.3 is selected from hydrogen, alkyl,
alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5, --NR.sub.6H,
--NH.sub.2, --COOH, --CO, --COOR.sub.S, --O--, --CHO, --S--,
--SO3H, --SO2, --SOCl.sub.2, halogen Cl, --Br, --I, --F),
--PR.sub.8R.sub.9, or --COCl.
18. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00031## in which each of
R.sub.1, R.sub.2, R.sub.3, R.sub.4, and R.sub.5, is selected from
hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl,
aryl, with or without hetero atoms, with or without substituent
groups including --OH, --SH, --NO.sub.2, --CN, --NR.sub.6R.sub.7,
--NR.sub.8H, --NH.sub.2, --COOH, --CO, --COOR.sub.S, --O--, --CHO,
--S--, --SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.10R.sub.11, or --COCl.
19. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00032## in which each of
R.sub.1, R.sub.2, and R.sub.3 is selected from hydrogen, alkyl,
alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5, --NR.sub.6H,
--NH.sub.2, --COOH, --CO, --COOR.sub.S, --O--, --CHO, --S--,
--SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl.
20. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00033## in which each of
R.sub.1, R.sub.2, and R.sub.3 is selected from hydrogen, alkyl,
alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5, --NR.sub.6H,
--NH.sub.2, --COOH, --CO, --COOR.sub.7, --O--, --CHO, --S--,
--SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl.
21. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00034## in which each of
R.sub.1, R.sub.2, R.sub.3, and R.sub.4, is selected from hydrogen,
alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.5R.sub.6, --NRH, --NH.sub.2,
--COOH, --CO, --COOR.sub.S, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.9R.sub.10, or --COCl.
22. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00035## in which each of
R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and R.sub.6 is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2, --COOH, --CO,
--COOR.sub.10, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.11R.sub.12,
or --COCl.
23. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00036## in which each of
R.sub.1, R.sub.2, R.sub.3, R.sub.4, and R.sub.5, is selected from
hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl,
aryl, with or without hetero atoms, with or without substituent
groups including --OH, --SH, --NO.sub.2, --CN, --NR.sub.6R.sub.7,
--NR.sub.8H, --NH.sub.2, --COOH, --CO, --COOR.sub.S, --O--, --CHO,
--S--, --SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.10R.sub.11, or --COCl.
24. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00037## in which each of
R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and R.sub.6 is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2, --COOH, --CO,
--COOR.sub.10, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.11R.sub.12,
or --COCl.
25. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00038## in which each of
R.sub.1, R.sub.2, R.sub.3, and R.sub.4, is selected from hydrogen,
alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.5R.sub.6, --NRH, --NH.sub.2,
--COOH, --CO, --COOR.sub.S, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.9R.sub.10, or --COCl.
26. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00039## in which each of
R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and R.sub.6 is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2, --COOH, --CO,
--COOR.sub.10, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --PR.sub.11R.sub.12, or --COCl.
27. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00040## in which each of
R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and R.sub.6 is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2, --COOH, --CO,
--COOR.sub.10, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), or --COCl.
28. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from an additive, said
additive having a structure formula: ##STR00041## in which each of
R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, R.sub.6, R.sub.7,
R.sub.8, and R.sub.9 is selected from hydrogen, alkyl, alkoxy,
alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or without hetero
atoms, with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.10R.sub.11, --NR.sub.12H, --NH.sub.2,
--COOH, --CO, --COOR.sub.13, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.14R.sub.15, or --COCl.
29. The method of claim 1, wherein: said metallic catalyst is a
metal salt.
30. The method of claim 1, wherein: said metallic catalyst is an
organometallic compound.
31. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from animal fatty acids.
32. The method of claim 1, wherein: at least some carbon used to
form said carbon nanotube is obtained from plant oils.
33. The method of claim 1, wherein: said carbon nanotube is
characterized by Bragg diffraction pattern peaks appearing at 2
theta (2.theta.) of approximately 26.degree., 43.5.degree..
34. The method of claim 1, wherein: said carbon nanotube is
characterized by Bragg diffraction pattern peaks appearing 2 theta
(2.theta.) of approximately 44.5.degree., 51.6.degree..
35. A method comprising a plurality of activities, comprising: via
a carbon nanotube, fabricating a composite adapted for use in
biomechanical devices; surgical implants; tissue-engineering
structures including bone, tendon, muscle, nerve, skin implants or
surrogates; wound-healing structures, or molecular capture devices
adapted for timed drug delivery, said carbon nanotube produced via
a tube control agent (TCA) and a metallic catalyst, at least some
carbon used to form said carbon nanotube obtained from starch,
bean, cloth, wood, plant, cellulose or cellulosic products, said at
least some carbon converted into powder by at least one of:
mechanical milling, biochemical reaction, and chemical
reaction.
36. A method comprising a plurality of activities, comprising: via
a carbon nanotube, fabricating a composite adapted for use in a
rotation part, said carbon nanotube produced via a tube control
agent (TCA) and a metallic catalyst, at least some carbon used to
form said carbon nanotube obtained from starch, bean, cloth, wood,
plant, cellulose or cellulosic products, said at least some carbon
converted into powder by at least one of: mechanical milling,
biochemical reaction, and chemical reaction.
Description
CROSS-REFERENCES TO RELATED APPLICATIONS
[0001] This application claims priority to, and incorporates by
reference herein in its entirety, pending U.S. Provisional Patent
Application Ser. No. 61/173,777 (Attorney Docket No. 1200-002),
filed 29 Apr. 2009.
BRIEF DESCRIPTION OF THE DRAWINGS
[0002] A wide variety of potential practical and useful embodiments
will be more readily understood through the following detailed
description of certain exemplary embodiments, with reference to the
accompanying exemplary drawings in which:
[0003] FIG. 1 shows a general schematic of an exemplary embodiment
of a reactor system 1000;
[0004] FIG. 2 shows a general schematic of an exemplary embodiment
of a reactor system 2000;
[0005] FIG. 3 shows a general schematic of a reactor using an
electric stove using a quartz tube and/or a ceramic tube adapted
for solid phase synthesis of carbon nanotubes;
[0006] FIG. 4 shows a Fourier Transform Infrared ("FtIR") spectrum
of three different TCA in which TCA 3 shows an absorption peak due
to a --CN group;
[0007] FIG. 5 shows a Field Emission Scanning Electron Microscopy
("FE-SEM") image of pyrolysis product using a TCA comprising a --CN
group (resin3);
[0008] FIG. 6 shows a FE-SEM image of a pyrolysis product using TCA
(resin 1 and 2) lacking a--CN group;
[0009] FIG. 7 shows a FE-SEM image of pyrolysis product using
additives carrying a --CN group (TCA 4);
[0010] FIG. 8 shows a FE-SEM image of nano carbon product from an
exemplary embodiment (using TCA containing --CN group, TCA 4)
having an outside diameter of approximately 600 nm and an inside
diameter of approximately 420 nm;
[0011] FIG. 9 shows a FE-SEM image of carbon nano product from an
exemplary embodiment (using. TCA containing additives comprising a
--CN group, TCA 4) having an outside diameter less than
approximately 1 nm;
[0012] FIG. 10 shows a FE-SEM image of a twisting nano carbon
product from an exemplary embodiment (using TCA containing additive
comprising a--CN group TCA 4);
[0013] FIG. 11 is a reference thermogravimetric analysis ("TGA")
data regarding heat resistant properties of a known carbon nano
tube product;
[0014] FIG. 12 illustrates TGA data for an exemplary embodiment of
nano carbon product using a TCA comprising a --CN group;
[0015] FIG. 13 shows a FE-SEM image of nano carbon structures of an
exemplary embodiment using a TCA comprising a --CN group;
[0016] FIG. 14 is an X-ray diffractogram of carbon nano structures
of the exemplary embodiment illustrated in FIG. 13;
[0017] FIG. 15 shows a FE-SEM image of nano carbon structures of an
exemplary embodiment using TCA comprising a --CN group;
[0018] FIG. 16 is an X-ray diffractogram of carbon nano structures
of the exemplary embodiment illustrated in FIG. 15;
[0019] FIG. 17 shows a FE-SEM image of nano carbon product of an
exemplary embodiment when additives carrying a --CN group were
used;
[0020] FIG. 18 is an X-ray diffractogram of nano carbon product of
the exemplary embodiment illustrated in FIG. 17;
[0021] FIG. 19 shows a FE-SEM image of nano carbon product of an
exemplary embodiment when additives carrying a --CN group were
used;
[0022] FIG. 20 is an X-ray diffractogram of nano carbon products of
the exemplary embodiment illustrated in FIG. 19;
[0023] FIG. 21 is a flowchart of an exemplary embodiment of a
method 21000;
[0024] FIG. 22 is an FtIR of TCA 4, which shows a --CN group;
[0025] FIG. 23 is a block diagram of an exemplary embodiment of a
reactor system 23000;
[0026] FIG. 24 is a table of thermogravimetric analysis data for
certain exemplary embodiments;
[0027] FIG. 25 shows a FE-SEM image of a wood powder raw material
of an exemplary embodiment carrying TCA;
[0028] FIG. 26 shows a FE-SEM image of nano carbon product of an
exemplary embodiment from the raw material described in FIG.
25;
[0029] FIG. 27 shows a FE-SEM image of a chemical top down, product
of the wood powder described in FIG. 25;
[0030] FIG. 28 shows a FE-SEM image of nano carbon product of an
exemplary embodiment from the raw material described in FIG. 27;
and
[0031] FIG. 29 shows effect of baking temperature on the nano
carbon product diameter for two different baking modes; gradual
baking mode and sudden baking mode.
DETAILED DESCRIPTION
[0032] Certain exemplary embodiments can comprise, via a tube
control agent ("TCA") and a metallic catalyst, producing a tube
shape nano carbon product. At least some carbon sources used to
form the tube shape nano carbon product can be obtained from a
plant, a cellulose product, and/or a cellulosic product. At least
some of the raw material can be converted into powder.
[0033] A carbon nano fiber is a nano carbon product having very
small diameter, which can be less than 5 nm or even less than 1 nm
and can be characterized by Bragg diffraction pattern peaks
appearing at 2 theta (2.theta.) of approximately 26.degree. and/or
43.5.degree.. A carbon nanotube is a nano carbon products disclosed
and characterized by Bragg diffraction pattern peaks appearing 2
theta (2.theta.) of approximately 44.5.degree. and/or 51.6.degree..
Another carbon nanotube is characterized by Bragg diffraction
pattern peaks appearing 2 theta of approximately 26.degree. and/or
43.5.degree.. These carbon nano materials can be prepared in a
solid phase by the pyrolysis and/or heating of the solid raw
materials both with a specific additive named as tube control agent
or tube control additive ("TCA"). A tube shape nano carbon product
growth process can comprise controlling the length of the tubes as
well as the tube diameter. FIG. 25 shows FE-SEM image of a raw
precursor made out of wood chips. FIG. 26 shows the resulting nano
carbon product from the raw material described in FIG. 25.
[0034] FIG. 27 shows an FE-SEM image of a chemical top down product
from the wood chips described in FIG. 25. A large bundle of wood,
such as observed in FIG. 25, can be torn off into small micro
fibrils as shown in FIG. 27.
[0035] FIG. 28 show the nano carbon product of the exemplary
embodiment from the raw material described in FIG. 27. A comparison
of FE-SEM image of FIGS. 26 and 28 confirmed that small size raw
materials gives small scale of nano carbon products.
[0036] In certain exemplary embodiments, the solid phase synthetic
process of a precursor comprised of solid carbon source, specific
tube control additive and solid catalyst can control the tube size
in terms of length and diameter.
[0037] The pyrolysis or heating process can be carried out in two
different modes: a slow or gradual heating process and a sudden
heating process. It is found that changing of heating mode will
change baking process; and sudden heating mode always gives rise to
longer length and larger diameter than gradual heating mode (FIG.
29 and FIG. 30).
[0038] Certain exemplary embodiments relate to nano technology, and
more particularly relate to a carbon nanotubes and carbon nano
fiber.
[0039] Techniques that have been developed to produce nanotubes in
sizeable quantities comprise arc discharge, laser ablation, high
pressure carbon monoxide (HiPCO), and/or chemical vapor deposition
(CVD). The CVD method has shown promise in terms of its price/unit
ratio. The CVD equipment and process can be plasma enhanced CVD
(PECVD), plasma remote CVD, and/or thermal CVD, etc. In certain
processes of CVD, the carbon source materials are thermally
decomposed (by the heat source or by plasma) into free radicals of
carbon, which then selectively adsorb onto the surface of selective
metallic catalyst(s) where the tube growth can occur. Thus, the
carbon source materials, first of all, can be molecules and/or
molecule clusters, which carry the chemical bonds or functional
groups, can be broken down into free radicals and remanufactured
into the tube that comprises carbon atoms arranged by sp2 or sp3
bonding systems. Certain carbon source materials utilized in the
research of carbon nanotubes are hydrocarbons including triple bond
material such as acetylene gas, double bond materials such as
unsaturated hydrocarbon materials, and/or single bond materials
such as saturated hydrocarbon materials and/or alcohols. Certain
exemplary CVD methods involve reacting a carbon-containing gas
(such as acetylene, ethylene, ethanol, etc.) with metal catalysts
(such as cobalt, nickel, iron and/or a combination of these such as
cobalt/iron or cobalt/molybdenum) at temperatures above
approximately 600.degree. C. These methods can be considered as gas
phase synthesis process in which the free radicals of carbon will
adsorb onto the surface of a catalyst already located on a support.
Thus, this process can also be called a catalytic support growth
process. In other processes, gas phase carbon sources are mixed
with vapor phase catalyst(s) in the high temperature zone of the
reactor. So the premix precursors, which are not solid as sometimes
seen in a catalytic growth process, can end up in products
comprising uncontrolled impurities of varied diameters; even in one
single tube besides residue metals, certain exemplary embodiments
can comprise non-tube products such as amorphous carbon. In certain
exemplary embodiments, efforts to achieve very pure carbon nanotube
such as single walled carbon nanotube (SWCNT) with gas phase plasma
CVD process can end up with a relatively low yield in a relatively
long reaction time due to slow feeding rate of gas precursor(s)
into the reaction chamber.
[0040] An alternative process that might overcome certain issues
found in the gas phase process can be denoted as a solid phase
synthetic process. Certain exemplary embodiments of the solid phase
synthetic process can comprise two methods; an arc discharge and a
laser ablation method. In the arc discharge method, an electric arc
is an electrical breakdown of a gas which produces an ongoing
plasma discharge, similar to the instant spark, resulting from a
current flowing through normally nonconductive media such as air.
An archaic term is the voltaic arc as used in the phrase "voltaic
arc lamp". The various shapes of electric arc are emergent
properties of nonlinear patterns of the current and the electric
field. The arc occurs in the gas-filled space between two
conductive electrodes (often made of carbon) and results in a
relatively high temperature, capable of melting or vaporizing
virtually anything. In the arc discharge process, a carbon anode
loaded with catalyst material (such as a combination of metals such
as nickel/cobalt, nickel/cobalt/iron, and/or nickel and/or a
transition element such as yttrium, etc.) is consumed in the arc
plasma. The catalyst and the carbon are vaporized, and the carbon
nanotube ("CNT") material is grown by the condensation of carbon
onto the condensed liquid catalyst. Sulfur compounds such as iron
sulfide, sulfur or hydrogen sulfides can be used as a catalyst
promoter to maximize the single walled nanotube ("SWNT") material
yield. When using certain exemplary methods based on arc discharge,
it can be difficult to increase the amount of vaporized carbon,
and/or can be difficult to control the process parameters of the
arc. In the arc the carbon rods can act as the feed materials and
the source (electrodes) for arc discharge. Accordingly, it can be
difficult to separately control these functions. This can result in
limited production of carbon nanotubes and in a product that can be
contaminated with other clustered carbon materials, causing a
relatively high cost of mass production. The cost of SWNT material
can be determined by production rate, yield, and raw materials
cost. The raw materials consist of a carbon source, a catalyst, and
promoters. Current modes of SWNT material production involve the
use of catalyst-packed graphite rods which are consumed in a direct
current ("DC") electric arc to produce soot that contains SWNT
material.
[0041] A variation of the packed rod technique can utilize the
catalyst as a molten metal in a small crucible onto which a
graphite rod is arced, thereby co-vaporizing carbon and catalyst to
form several grams of SWNT material per operation. The product of
the arc-based production methods contains SWNT material that is
substantially coated with substantially amorphous carbon, as well
as with other contaminants, which can comprise amorphous and/or
graphitic carbon particles, carbon-coated metal catalyst particles,
and/or traces of fullerenes-C.sub.60, C.sub.70, etc. Separation
schemes have been devised to remove the contaminant which allow
limited (1.about.10%) recovery of relatively pure carbon nanotubes.
Relatively pure SWNT material can be produced from untreated
bituminous coal, but can have a twofold to fourfold reduction in
purity, such as from transition metal impurities (e.g., such as
from pyrite in bituminous coal), which can contribute a synergistic
catalytic effect. In certain exemplary embodiments, it might be
possible to produce SWNT material from pyrite rich bituminous coal
without adding any separate catalyst. However, the presence of
sulfur can decrease the yield of SWNT compared to embodiments that
substantially do not comprise sulfur.
[0042] CNT can be synthesized by laser ablation such as by using a
laser to ablate a composite block of graphite mixed with catalytic
metal. The catalytic metal can comprise Co, Nb, Pt, Ni, Cu, and/or
a combination thereof. The composite block can be formed by making
a paste of graphite powder, carbon cement, and the catalytic metal.
The paste can be placed in a cylindrical mold and baked for several
hours. After solidification, the graphite block can be placed
inside an oven with a laser pointed at it, and an inert gas such as
Ar gas can be pumped along the direction of the laser point. The
oven temperature can be approximately 1200.degree. C. As the laser
ablates the target, carbon nanotubes form and are carried by the
gas flow onto a cool copper collector. Like carbon nanotubes formed
using the electric-arc discharge technique, carbon nanotube fibers
can be deposited in a relatively haphazard and/or tangled
fashion.
[0043] Although certain exemplary methods can produce relatively
large quantities of nanotubes, their cost can be a barrier to
large-scale applications. Further, these naturally occurring
varieties, because of the highly uncontrolled environment in which
the carbon nanotubes are produced, can be irregular in size and/or
quality, lacking the high degree of uniformity to meet certain
objectives of research and/or industry. Certain exemplary
embodiments can produce these nanotubes at low cost and with
suitable purity and physical properties (e.g., controlled length
and chirality) for applications in a high volume industrial
process.
[0044] When making carbon nanotubes in the gas phase, the diameter
and/or the length of the tube can be difficult to control. In the
process of making carbon nanotubes using plasma or sophisticated
energy sources such as an e-beam and/or a laser beam, the product
cost can be relatively high to produce fine carbon fibers and/or
several different kinds of carbon nanotubes. Certain exemplary
embodiments can comprise a production method of producing a
combination of (1) a polymer material that disappears upon thermal
decomposition and (2) carbon precursor polymers. The polymer
material can be thermally decomposed. Carbon is formed from the
carbon precursor polymers. The foregoing combination can comprise
micro-capsules that include a shell of the carbon precursor
polymers on the polymer material that disappears upon thermal
decomposition. The thermal decomposing and the forming can be
performed by baking the micro-capsules. The micro-capsules can be
prepared by an interfacial chemical technique. The micro
encapsulation technique can be relatively complicated and expensive
for large volume production as the raw material preparation needs
more complicated steps. Overall, these processes can give rise to a
relatively low yield of carbon products and/or CNT products.
[0045] Certain exemplary embodiments can synthesize carbon
nanotubes and related nano materials having a relatively high
yield. Certain exemplary embodiments can provide a solid phase
synthesized carbon nano fiber and/or nanotube by the pyrolysis of
solid carbon source mixed with tube control agent under unoxidizing
atmosphere. The process can have some advantages and benefits over
other solid phase synthetic process using arc discharge and laser
ablation technique in terms of reaction yield improvement and large
production scale capability.
[0046] In order to achieve a relatively high yield of tube shape
products, first, the process can produce a relatively high yield of
pyrolysis product and/or the portion of tube shape components in
the pyrolysis product can be high. The yield can be determined as
the weight percentage of the pyrolysis product obtained from the
original weight of the precursor at the end of pyrolysis process.
The terminology of "high yield" can be defined as a yield greater
than approximately 20%. Other kinds of precursor(s) containing a
relatively high portion of aromatic systems such as polystyrene and
its copolymers can give a relatively poor yield of pyrolysis
products. Certain exemplary embodiments can combine the factors
providing a relatively high yield of pyrolysis products and the
factors providing a relatively high yield of tube shape products in
order to achieve a relatively high yield of carbon nanotubes.
[0047] Certain exemplary embodiments provide a material set that
can help to form controllable carbon nanotube products in terms of
uniformity, purity, and/or relatively high conductivity. The
specific solid precursor can be composed of 3 components: a) carbon
source from specific plant and/or plant products, such as a tree
from a tropical area, b) specific tube control additives (TCA), and
c) a metallic catalyst. These three component combination can
efficate a solid phase process of producing carbon nanotubes.
[0048] The solid phase synthesized carbon nanotubes and carbon nano
fibers can be produced by heating of solid raw materials in a
substantially oxygen free environment utilizing precursor(s)
comprising a selected combination of carbon sources, specific tube
control agent and/or one or more metallic catalysts, etc. In
certain exemplary embodiments, such components can form a
harmonical combination adapted to form a unique precursor capable
of forming desirable carbon nanotube products. The specific TCA can
be an important factor as the TCA can effectively provoke the
adsorption of free carbon radicals onto metallic catalyst
molecules. These functions can exist on separated molecules and/or
can co-exist in a single molecule.
[0049] In order to work with a selected TCA, certain kinds of solid
carbon sources can be used. The solid carbon sources can be
selected from cellulose products from the trees, plants, vegetables
found in tropical area in the world including Asia, Africa, and/or
South America, etc. These cellulose products can be but not limited
to starch, wood, paper, cloth, bean, cotton, and the like. The
starch, which can form tube shape of nano carbon products, can
comprise rice starch, potato starch, corn starch, wheat starch, and
the like. The cellulosic wood products can be pine wood powder,
cedar wood powder, bamboo wood powder, paddy shell powder, coconut
shell, and the like. The cellulosic sources can be soy bean, green
bean, red bean, black bean, coffee bean, corn and the like or a
combination of different bean source. The carbon sources can be
selected from natural products other than cellulosic sources such
as fatty acid from animals, vegetable oils, biodiesel oils,
jetropha curcas oil, coconut oils, sesame seed oils, soy bean oils,
eucalyptic leaves containing eucalyptic oils. Such oil stuffs need
to be stabilized on a substrate by adsorbing on a solid carbon
source before entering the reaction chamber.
[0050] The cellulose carbon sources can be formatted into a powdery
format. The powdery format of carbon source materials can be
achieved by a mechanical milling (this can be called as physical
top-down process), a biochemical process, or a chemical process
(this can be called as chemical top-down process). For the second
case, a biochemical enzyme can be utilized to convert the powder
products into nano powder products by a chemical reaction of enzyme
on cellulosic materials. For the third case, some specific
chemicals can be added to split the large accumulation of
cellulosic substance into much smaller micro fibril products. Thus,
it is working as a chemical top-down process in a comparison with a
physical top-down process utilizing mechanical milling
[0051] The tube control agent molecules can be selected from a
group of chemicals having two specific functional groups. The first
functional group can have a relatively strong interaction with
metallic element in the metallic catalyst. The second functional
group can have a relatively strong adhesion with carbon source
molecules. The tube control agent molecules can be selected from a
group of chemicals having specific functional groups as indicated
below
##STR00001##
in which the formula comprises a 3 member ring, 4 member ring, 5
member ring, 6 member ring, 7 member ring, or 8 member ring having
substituent groups including hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, or aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.1R.sub.2, --NR.sub.3H, --NH.sub.2,
--COOH, --CO, --COOR.sub.4, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.5R.sub.6, --COCl. These member rings are saturated and
unsaturated, n=1, . . . 6. These member rings can be benzene,
napthalene, anthracene, perylene, perinone
[0052] The tube control agent itself can be a carbon source and/or
can be physically or chemically doped onto the carbon source
molecules. The tube control agent can work as an effective hook
linking metal catalyst molecules with carbon sources molecules. The
above described tube control agents can be used alone or it can be
used together with specific additives such as described in (5) (6)
(7) (8) (9) (10) (11)
##STR00002##
[0053] in which R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5 can be
metal, hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with and without hetero atoms, with and
without substituent groups, which can comprise --OH, --SH,
--NO.sub.2, --CN, --NR.sub.6R.sub.7, --NR.sub.8H, --NH2, --COOH,
--CO, --COOR.sub.S, --O--, --CHO, --S--, --SO.sub.3H, --SO.sub.2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.10R.sub.11R.sub.12, R.sub.13, R.sub.14, and/or --COCl.
Each of R.sub.6, R.sub.7, R.sub.8, R.sub.9, R.sub.10, R.sub.11,
R.sub.12, R.sub.13, R.sub.14, can be functional groups which can
contribute to physical and/or chemical properties of TCA and thus,
can contribute to the success of making carbon nano fiber and tube,
for example, by increasing adsorption power and/or enhancing
interaction between carbon sources, catalyst and/or TCA; the ring
can be a 3, 4, 5, 6, 7, or 8 member ring, an unsaturated or
saturated ring. Examples of additives can be cited as but not
limited to those enumerated hereinbelow:
##STR00003##
in which R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, R.sub.6,
R.sub.7 can be metal, hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, aryl, with and without hetero atoms,
with and without substituent groups, which can comprise --OH, --SH,
--NO.sub.2, --CN, --NR.sub.8R.sub.9, --NR.sub.10H, --NH2, --COOH,
--CO, --COOR.sub.11, --O--, --CHO, --S--, --SO.sub.3H, --SO.sub.2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.12R.sub.13, R.sub.14, R.sub.15, R.sub.16, and/or --COCl,
and/or the like. Each of R.sub.8, R.sub.9, R.sub.10, R.sub.11,
R.sub.12, R.sub.13, R.sub.14, R.sub.15, R.sub.16 can be functional
groups which can contribute to physical and/or chemical properties
of TCA and thus, can contribute to the success of making carbon
nano fiber and tube, for example, by increasing adsorption power
and/or enhancing interaction between carbon sources, catalyst,
and/or TCA.
[0054] Examples of these compounds can be cited as:
TABLE-US-00001 acetonitrile pine wood resin cedar wood oil 1
Poly(styrene-co-acrylonitrile) 18,286-9 2 Poly acrylonitrile 3 Poly
3-methylenecyclobutene-
www.springerlink.com/index/U818173063883084.pdf 1-carbonitrile 4
Poly(acrylonitrile-co- 41890-0 butadiene), amine terminated 5 Poly
3-methylenecyclobutene-
www.springerlink.com/index/U818173063883084.pdf 1-carbonitrile 6
Poly(acrylonitrile-co- 41890-0 butadiene), amine terminated 7
copo(acrylonitrile-butadiene- ABS resin styrene) 8 Phthalonitrile
and its derivatives 9 2,2'-Azobisisobutyronitrile Aldrich cat No
44,109-0 10 4,4-Azobis(4-cyanovaleric acid) Aldrich cat No 11,816-8
11 1,1' Azobis(cyclo- Aldrich cat No 38,021-0 hexanecarbonitrile)
12 acetonitrile Aldrich cat No 48,521-7 13 Acrylonitrile monomer 14
2-acetoxy-3-butenenitrile Aldrich cat No 27,962-5 15 1-Cyanovinyl
acetate 22,603-3 16 5-Acetoxymethyl-2-amino-3- 86,162-6
cyanopyrazine 17 Acetoxyphenylacetonitrile 42,019-0 18 2-Acetoxy-4-
41,996-6 phenylbutyronitrile 19 5-acetyl-2-amino-4-(2- 45,148-7
furanyl)-6-methyl-4 H- pyran-3-carbonitrile 20 Nipecotamic Aldrich
catalog N810-5 21 4-hydroxy quinazoline Aldrich Catalog number
H5,760-2 22 4-Hydroxypyrazolo[3,4- Aldrich Catalog number H5,660-6
d]pyrimidine 23 Primuline Aldrich Catalog number 20,686-5 24
Phosphonitrilic chloride Aldrich Catalog number 23,028-6 trimer 25
Phosphorus tribromide Aldrich Catalog number 25,653-6 26
Hexyltributylphosphonium Aldrich Catalog number 35,933-5 bromide 27
Hexyltriethylammonium Aldrich Catalog number 30,144-2 bromide 28
Lignin from tree
[0055] Carbonitrile compounds can be polymers of
3-methylenecyclobutene-1-carbonitrile, pine wood resin containing
--CN, polymer of 2-methyl, 3-methylenecyclobutene-1-carbonitrile,
and/or any polymers comprising a carbonitrile functional group
[0056] Carbonitrile polymeric precursors for the synthesis of
carbon nanotube may contain plasticizers such as Dibutyl phthalate,
Di-2-ethylhexyl phthalate, Dicyclohexyl phthalate, Butylbenzyl
phthalate, Diisodecyl phthalate, Diisononyl phthalate, Di-n-hexyl
azelate, Di-2-ethylhexyl adipate, Acetyl tributyl citrate,
Acetyl-tri-2-ethylhexyl citrate, Diphenyl-2-ethylhexyl phosphate,
Diisononyl phthalate, 1,2-Cyclohexane dicarbonic acid-diisononyl
ester, Adipic acid polyester with 1,3-butanediol and
1,6-hexanediol, di-n-octyl tin, and the like.
[0057] Besides carbonitrile compounds as cited above, electron
donor molecules such as amino compound, phosphonium compound,
ammonium compounds can also be effective TCA to produce tube shape
nano carbon products
[0058] The foregoing implementations can be described by reference
to FIGS. 1-4.
EXAMPLES
Example 1
[0059] Measurement of Fourier transform infrared spectroscopy
(FtIR) chart of three different pine wood resin 1, 2, 3 Pine wood
resin 1, 2, 3 were obtained from different sources. FIG. 4 shows
FtIR charts of these 3 different kinds of pine wood resins. The
FtIR chart of resin 1 and 2 didn't show any absorption peaks at the
vicinity of approximately 1050 cm.sup.-1, representing --CN group.
This data reveals that the resin 3 is the only one which does carry
carbonitrile --CN group on its molecule. FIG. 22 shows FtIR of
another TCA compound. This TCA when added into the solid precursor
shows tube shape nano products in the exemplary of embodiment
Example 2
[0060] Preparation of the precursor using resin 3 carrying --CN
group in the molecule. Approximately one (1) g of FeCl.sub.3 and 10
g of TCA number 9 in the list were dissolved in a mixture of a
solvent containing ten (10) g of deionized water and five (5) g of
methanol. Then approximately six (6) g of pine wood resin were
added into the solution and stirred at room temperature for
approximately thirty (30) minutes, then heated up to approximately
one hundred degree Celsius (100.degree. C.) for approximately a
further ninety (90) minutes to achieve a light brown solid
powder.
[0061] FIG. 1 shows a general schematic of an exemplary embodiment
of a reactor system 1000, which can be for use in solid phase
synthesis of carbon nanotubes. Reactor system 1000 can use a gas
stove 1300 for a solid phase synthesis of carbon nanotubes. Reactor
system 1000 can comprise a raw material holder 1200. Carbon sources
can be placed in raw material holder 1200. Upon heating, the carbon
sources can evolve gases through an outgases inlet 1100. A valve
1400 can be opened to allow a vacuum pump 1500 to withdraw gases
from outgases inlet 1100.
Example 3
[0062] Synthesis of Carbon Nanotubes in a Solid Phase using
precursor containing --CN group (resin 3). The solid raw materials
described in the Example 2 were weighed into a quartz tube and then
inserted into the reaction chamber, as shown in FIG. 1, which was
pre-heated to approximately nine hundred degree Celsius
(900.degree. C.) and filled with N.sub.2 gas at the flow rate of
approximately 2.5 liters/minute. Then, the heating inside the
reaction chamber was started and the heating was continued for
approximately two (2) hours. Afterward, the positive heating was
stopped and a flow of N.sub.2 gas was continued until the
temperature of the chamber dropped to approximately room
temperature. The quartz tube was removed and the black product
inside the quartz tube was collected. The black product showed a
significant increase of magnetic properties, and was tested. The
results of the tests are shown by the FE-SEM, in FIG. 5. A tube
product was obtained in this example.
[0063] FIG. 2 shows a general schematic of an exemplary embodiment
of a reactor system 2000, which can utilize an electric stove for a
solid phase synthesis of carbon nanotubes. The reactor can
comprise: [0064] an oven 1; [0065] an oven entire cover 1.1; [0066]
a heat resistant layer 1.2; [0067] a coil heater 1.4; [0068] a heat
controller 1.5; [0069] a pyrex glass annealing chamber 2; and/or
[0070] a neck connector 3.
[0071] Pyrex glass annealing chamber 2 can be described via a first
dimension 2200, a second dimension 2300, a third dimension 2400, a
fourth dimension 2500, and/or a sixth dimension 2600. Each of first
dimension 2200, second dimension 2300, third dimension 2400, fourth
dimension 2500, and/or sixth dimension 2600 can be any suitable
dimension for synthesis of carbon nanostructures. For example,
first dimension 2200 can be approximately, in mm, 4, 5.138, 8.28,
10.71, 12.5, 14.75, 18, 21.758, 41.6 and/or any value or subrange
therebetween. For example, each of second dimension 2300, third
dimension 2400, fourth dimension 2500, and/or sixth dimension 2600
can be approximately, in cm, 2, 3.135, 4, 5.984, 6.9, 8.247, 10.76,
12, 12.109, 12.5, 14.834, 15.875, 16, 22.4, 27.676, 32, 38.621, 40,
45.6, 51.237, 66.087, 76, 80, and/or an value or subrange
therebetween,
[0072] FIG. 3 shows a general schematic of a reactor using an
electric stove using a quartz tube and/or a ceramic tube for a
solid phase synthesis of carbon nanotubes, which can comprise one
or more mass flow controllers, an unoxidizing gas inlet, a furnace,
a quartz tube, a temperature controller, a cold trap, and/or an
absorbent.
Comparison Example 1
[0073] Examples 2 and 3 were repeated except that resin 1 was used
instead of resin 3 (as referenced in FIG. 4). The resultant Field
Emission Scanning Electron Microscope (FE-SEM) micrograph is seen
at reference numeral 400 in FIG. 6, from which it is seen that the
carbon nanotubes were not synthesized. Rather, fine particles of
carbon were synthesized. From this it can be concluded that resin
3, which carries the functional group --CN is effective as a tube
forming agent.
Example 4
[0074] Preparation of the precursor using resin 1 (as referenced in
FIG. 4) carrying substantially no --CN group in the molecule added
with additive carrying --CN group in the molecule. Repeat
Comparison Example 1 except that approximately two (2) g of TCA 4
(as indicated by FtIR chart illustrated in FIG. 22) was added
during the process of making solid precursor with non-CN group
resin 1 (as referenced in FIG. 4). The FE-SEM picture of the
pyrolysis product from Example 4 is shown in FIG. 7. The TCA 4
additive which carries the --CN group can help a precursor which
doesn't carry --CN group to form the tube product. Thus --CN group
can be the precursor to provoke the formation of carbon
nanotube.
[0075] FIG. 8 shows a FE-SEM image of carbon tube having outside
diameter of approximately 600 nm and inside diameter of
approximately 420 nm. FIG. 9 shows a FE-SEM image of carbon
nanotube having outside diameter less than approximately 1 nm. FIG.
10 shows a FE-SEM image of a twisting carbon nanotube of an
exemplary embodiment. All of these products are resulting of using
TCA comprising a --CN group.
[0076] Specific precursor for fabrication of carbon nanotube can be
comprised of specific carbon sources from plants and vegetables
grown in a specific geography, tube shape control additives (TCA),
and metallic catalysts, in which the carbon nanotubes are
fabricated into ultra high-strength nanofibers that can be woven,
knitted, sewn, interlaced, interlinked, netted, spun, spiraled,
twisted, looped, wet laid, laminated, veneered, thermoplasticized,
and/or gas phase-, chemical-, sputter- and/or vapor-deposited to
form materials and items including armor, coverings, and/or
components for persons, vehicles and structures, including for
protection against radiation, chemical, and/or biological agents;
fabricated into adhesive surfaces; fabricated into apparel,
footwear, and/or fabrics used for tarps, weather-resistant
coverings, and/or sails including ultraviolet radiation protection;
embedded into substrates for acoustic, infrared, ultraviolet,
and/or other electromagnetic radiation detection; embedded in
substrates to form tires, railroad bogies, and/or other friction
control and/or vibration control devices; fabricated into
load-bearing lines for use in parachutes, draglines, cargo
containers, netting, connecting lines and/or moorings for
land-based, aquatic, aerial, and/or outer space applications;
fabricated into structures for load-bearing and/or retention
applications in construction, including buildings, scaffolds,
marine vessel hulls, components, and/or fittings; aircraft and/or
aerospace fuselages and/or structures, and/or land-based vehicle
components, including body parts, engine components, and/or brake
linings; fabricated into composites used in biomechanical devices
and surgical implants and/or tissue-engineering structures
including bone, tendon, muscle, nerve, and/or skin implants and/or
surrogates, wound-healing structures, molecular capture devices for
timed drug delivery; fabricated into nano-cantilevers for
biosensing, cell growth, and/or orthopedic, vascular, and/or neural
prostheses; fabricated into filters, barriers, and/or wipes;
embedded into sheets and/or substrates as nanowires, ultrathin
films, photon detectors for the purpose of conducting electricity
and/or acting as batteries, membrane fuel cells, supercapacitors,
superconductors, electromagnetic and/or electro-optical actuators,
and/or microelectromechanical devices (e.g., for use in magnetic
resonance imaging machines, magnetic levitation trains, and/or
electric transmission lines); fabricated into sheets or structures
with variable optical properties; embedded into sheets for use as
heat conductors, heat sinks, high strength building and reinforcing
material, automotive, marine, and/or aviation and/or aerospace
panels; fabricated into tubular or I-beam cross sectional items for
use as conduits, structural members, and/or the like.
[0077] X-Ray diffraction (XRD) pattern can be one way to identify
the crystal structure of a solid. In certain exemplary embodiments,
tube diameters that are less than approximately 5 nm gives rise to
2 theta of approximately 25-26.degree., 43.5.degree.. Otherwise
tube diameter greater than approximately 15 nm gives rise to XRD
peaks at 2 theta of approximately 44.5.degree. and 51.6.degree..
XRD is one method to identify materials.
[0078] FIG. 11 is a reference TGA data regarding heat resistant
properties of a known carbon nano tube product (see, e.g.,
http://www.azonano.com/Details.asp?ArticleID=2037#_Catalytic_Activity).
[0079] FIG. 12 is a graph of thermogravimetric-differential thermal
analysis for an exemplary embodiment of carbon nanotubes that were
produced using additives comprising a CN group. FIG. 12 indicates
that certain exemplary carbon nanotubes produced using additives
comprising a CN group show at least 61.76% Residue at approximately
1400.degree. C.
[0080] FIG. 13 shows a FE-SEM image of carbon nano structures of an
exemplary embodiment. FIG. 14 is an X-ray diffractogram of carbon
nano structures of the exemplary embodiment illustrated in FIG. 13.
FIG. 15 shows a FE-SEM image of carbon nano structures of an
exemplary embodiment.
[0081] FIG. 16 is an X-ray diffractogram of carbon nano structures
of the exemplary embodiment illustrated in FIG. 15. FIG. 17 shows a
FE-SEM image of carbon nanotubes of an exemplary embodiment. FIG.
18 is an X-ray diffractogram of carbon nanotubes of the exemplary
embodiment illustrated in FIG. 17. FIG. 19 shows a FE-SEM image of
carbon nanotubes of an exemplary embodiment. FIG. 20 is an X-ray
diffractogram of carbon nanotubes of the exemplary embodiment
illustrated in FIG. 19.
[0082] Certain exemplary carbon nano products can be used as an
electron source, such as for electron microscopy, field emission
lighting, x-ray source, space propulsion, traveling wave tube
amplifiers, air remediation, water remediation, and/or cold field
emission, etc. Properties of carbon nano products can comprise a
relatively small tip radii (and relatively small source size),
relatively high electrical conductivity, relatively high melting
point, and/or resistance to electromigration under an applied
electric field. Carbon nanotube electron point sources can be
relatively stable, with relatively high brightness, relatively low
energy spread, and relatively low noise. Certain exemplary
embodiments can be adapted to produce emitter arrays that can
deliver relatively high current beams at relatively high
frequencies.
[0083] FIG. 21 is a flowchart of an exemplary embodiment of a
method 21000. At activity 21100, carbon can be obtained from a
carbon source. For example, the carbon can be obtained from one or
more of animal fatty acids, plant oils, a starch, a bean bearing
plant, cloth, wood, a plant, cellulose and/or a cellulosic product,
etc.
[0084] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00004##
in which each of R.sub.1, R.sub.2, and R.sub.3 is selected from
hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl,
aryl, with or without hetero atoms, with or without substituent
groups including --OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5,
--NR.sub.6H, --NH.sub.2, --COOH, --CO, --COOR.sub.7, --O--, --CHO,
--S--, --SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl.
[0085] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00005##
in which R is selected from hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.2R.sub.3, --NR.sub.4H, --NH.sub.2,
--COOH, --CO, --COOR.sub.5, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.6R.sub.7, or --COCl.
[0086] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00006##
in which each of R.sub.1 and R.sub.2 is selected from hydrogen,
alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.3R.sub.4, --NR.sub.5H,
--NH.sub.2, --COOH, --CO, --COOR.sub.6, --O--, --CHO, --S--,
--SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.7R.sub.8, or --COCl.
[0087] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00007##
in which each of R.sub.1, R.sub.2, and R.sub.3 is selected from
hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl,
aryl, with or without hetero atoms, with or without substituent
groups including --OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5,
--NR.sub.6H, --NH.sub.2, --COOH, --CO, --COOR.sub.S, --O--, --CHO,
--S--, --SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl.
[0088] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00008##
in which each of R.sub.1, R.sub.2, R.sub.3, R.sub.4, and R.sub.5,
is selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.6R.sub.7, --NR.sub.8H, --NH.sub.2, --COOH, --CO,
--COOR.sub.9, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.10R.sub.11,
or --COCl.
[0089] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00009##
in which each of R.sub.1, R.sub.2, and R.sub.3 is selected from
hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl,
aryl, with or without hetero atoms, with or without substituent
groups including --OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5,
--NR.sub.6H, --NH.sub.2, --COOH, --CO, --COOR.sub.7, --O--, --CHO,
--S--, --SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl
[0090] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00010##
in which each of R.sub.1, R.sub.2, and R.sub.3 is selected from
hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl,
aryl, with or without hetero atoms, with or without substituent
groups including --OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5,
--NR.sub.6H, --NH.sub.2, --COOH, --CO, --COOR.sub.S, --O--, --CHO,
--S--, --SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl.
[0091] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00011##
in which each of R.sub.1, R.sub.2, R.sub.3, and R.sub.4, is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.5R.sub.6, --NR.sub.7H, --NH.sub.2, --COOH, --CO,
--COOR.sub.S, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.9R.sub.10, or
--COCl.
[0092] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00012##
in which each of R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and
R.sub.6 is selected from hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2,
--COOH, --CO, --COOR.sub.10, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.11R.sub.12, or --COCl.
[0093] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00013##
in which each of R.sub.1, R.sub.2, R.sub.3, R.sub.4, and R.sub.5,
is selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.6R.sub.7, --NR.sub.8H, --NH.sub.2, --COOH, --CO,
--COOR.sub.9, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.10R.sub.11,
or --COCl.
[0094] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00014##
in which each of R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and
R.sub.6 is selected from hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2,
--COOH, --CO, --COOR.sub.10, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.11R.sub.12, or --COCl.
[0095] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00015##
in which each of R.sub.1, R.sub.2, R.sub.3, and R.sub.4, is
selected from hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl,
cycloalkylenyl, aryl, with or without hetero atoms, with or without
substituent groups including --OH, --SH, --NO.sub.2, --CN,
--NR.sub.5R.sub.6, --NR.sub.7H, --NH.sub.2, --COOH, --CO,
--COOR.sub.S, --O--, --CHO, --S--, --SO3H, --SO2, --SOCl.sub.2,
halogen (--Cl, --Br, --I, --F), --N.dbd.N--, --PR.sub.9R.sub.10, or
--COCl.
[0096] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00016##
in which each of R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and
R.sub.6 is selected from hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2,
--COOH, --CO, --COOR.sub.10, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.11R.sub.12, or --COCl.
[0097] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00017##
in which each of R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5, and
R.sub.6 is selected from hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.7R.sub.8, --NR.sub.9H, --NH.sub.2,
--COOH, --CO, --COOR.sub.m, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.11R.sub.12, or --COCl.
[0098] In certain exemplary embodiments, at least some carbon used
to form the carbon nanotube is obtained from an additive, the
additive having a structure formula:
##STR00018##
in which each of R.sub.1, R.sub.2, R.sub.3, R.sub.4, R.sub.5,
R.sub.6, R.sub.7, R.sub.8, and R.sub.9 is selected from hydrogen,
alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.10R.sub.11, --NR.sub.12H,
--NH.sub.2, --COOH, --CO, --COOR.sub.13, --O--, --CHO, --S--,
--SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.14R.sub.15, or --COCl.
[0099] At activity 21200, a TCA can be obtained. In certain
exemplary embodiments, the TCA can have a structure formula:
##STR00019##
in which each of R.sub.1, R.sub.2, and R.sub.3 is selected from
hydrogen, alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl,
aryl, with or without hetero atoms, with or without substituent
groups including --OH, --SH, --NO.sub.2, --CN, --NR.sub.4R.sub.5,
--NR.sub.6H, --NH.sub.2, --COOH, --CO, --COOR.sub.7, --O--, --CHO,
--S--, --SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.8R.sub.9, or --COCl.
[0100] In certain exemplary embodiments, the TCA can have a
structure formula:
##STR00020##
in which each of R.sub.1 and R.sub.2 is selected from hydrogen,
alkyl, alkoxy, alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or
without hetero atoms, with or without substituent groups including
--OH, --SH, --NO.sub.2, --CN, --NR.sub.3R.sub.4, --NR.sub.5H
--NH.sub.2, --COOH, --CO, --COOR.sub.6, --O--, --CHO, --S--,
--SO3H, --SO2, --SOCl.sub.2, halogen (--Cl, --Br, --I, --F),
--N.dbd.N--, --PR.sub.7R.sub.8, or --COCl.
[0101] In certain exemplary embodiments, the TCA can have a
structure formula:
##STR00021##
in which R.sub.1 is selected from hydrogen, alkyl, alkoxy,
alkylenyl, cycloalkyl, cycloalkylenyl, aryl, with or without hetero
atoms, with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.2R.sub.3, --NR.sub.4H, --NH.sub.2,
--COOH, --CO, --COOR.sub.5, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.6R.sub.7, or --COCl.
[0102] In certain exemplary embodiments, the TCA can have a
structure formula:
##STR00022##
in which the formula comprises a 3 member ring, 4 member ring, 5
member ring, 6 member ring, 7 member ring, or 8 member ring having
substituent groups including hydrogen, alkyl, alkoxy, alkylenyl,
cycloalkyl, cycloalkylenyl, or aryl, with or without hetero atoms,
with or without substituent groups including --OH, --SH,
--NO.sub.2, --CN, --NR.sub.1R.sub.2, --NR.sub.3H, --NH.sub.2,
--COOH, --CO, --COOR.sub.4, --O--, --CHO, --S--, --SO3H, --SO2,
--SOCl.sub.2, halogen (--Cl, --Br, --I, --F), --N.dbd.N--,
--PR.sub.5R.sub.6, --COCl, wherein member rings are saturated and
unsaturated with a value of n between 1 and 6; the member rings
comprising benzene, napthalene, anthracene, perylene, or
perinone.
[0103] At activity 21300, a catalyst, such as a metallic catalyst
can be obtained. In certain exemplary embodiments the metallic
catalyst can comprise a metal salt and/or an organometallic
compound.
[0104] At activity 21400, the carbon can be converted to a powder.
For example, the carbon can be converted to a powder via one or
more of mechanical milling, biochemical reaction, and/or chemical
reaction, etc.
[0105] At activity 21500, raw materials comprising the carbon, the
TCA, and/or the catalyst can be heated.
[0106] At activity 21600, the carbon can be converted to a carbon
nano structure such as a structure comprising a carbon nanotube, a
carbon nano fiber, and/or a functionalized nano carbon. In certain
exemplary embodiments, via a solid phase synthetic process
utilizing the TCA and the metal catalyst, a length and/or diameter
of the carbon nanotube, the carbon nano fiber, and/or the
functionalized nano carbon can be controlled. Certain exemplary
embodiments result in a relatively short carbon nanotube without
utilizing an X-Ray or an electron beam ("E beam").
[0107] In certain exemplary embodiments, the carbon nanotube can be
characterized by
[0108] Bragg diffraction pattern peaks appearing at 2 theta
(2.theta.) of approximately 26.degree., 43.5.degree.. In certain
exemplary embodiments, the carbon nanotube is characterized by
Bragg diffraction pattern peaks appearing 2 theta (2.theta.) of
approximately 44.5.degree., 51.6.degree..
[0109] At activity 21700, an item can be fabricated. For example,
via a carbon nanotube, one or more of the following items can be
fabricated: [0110] components adapted for use as armor or a
covering that at least partially resists penetration by a
projectile, radiation, chemical agents, or biological agents;
[0111] adhesive surfaces; [0112] apparel, footwear, or fabrics
adapted for use as a tarp, weather-resistant covering, or sail;
[0113] substrates adapted for acoustic, infrared, ultraviolet, or
other electromagnetic radiation detection; [0114] substrates
adapted to form tires, railroad bogies, friction control, or
vibration control devices; [0115] load-bearing lines adapted for
use in parachutes, draglines, cargo containers, netting, or
connecting lines; [0116] moorings adapted for land-based, aquatic,
aerial, or outer space applications; [0117] structures adapted for
load-bearing or retention applications in construction, including
buildings, scaffolds, marine vessel hulls, components, or fittings;
[0118] construction materials adapted for use in structures; [0119]
metallic alloys adapted for use in structures, the metallic alloys
comprising nano carbon structures and at least one metal; [0120]
ceramic composites adapted for use in structures, the ceramic
composites comprising nano carbon structures and at least one
ceramic material; [0121] a structure comprising a heat resistant
composite adapted to resist thermal decomposition to at least 1500
degrees Celsius; [0122] superconductor composites adapted for use
in structures, the superconductor composites prepared at
temperature higher than 1500 degrees Celsius, the superconductor
composites comprising nano carbon structures and at least one
superconducting material; [0123] high temperature composites
adapted for use in structures; [0124] aircraft or aerospace
fuselages or structures, or land-based vehicle components,
including body parts, engine components, or brake linings; [0125]
rotation parts adapted for use in at least one of: [0126] vehicles;
[0127] transportation devices, [0128] rotating equipment; or [0129]
rotating tools; [0130] bearings; [0131] composites adapted for use
in paints adapted to resist scratches and wear caused by an impact
or collision; [0132] colorants adapted for use in ceramic
coloration process, processing at high heat condition; [0133]
composites adapted for use in brick; [0134] composites adapted for
use in biomechanical devices; surgical implants; tissue-engineering
structures including bone, tendon, muscle, nerve, skin implants or
surrogates; wound-healing structures, or molecular capture devices
adapted for timed drug delivery; [0135] nano-cantilevers adapted
for biosensing, cell growth, or orthopedic, vascular, or neural
prostheses; [0136] filters, barriers, or wipes; [0137] sheets,
substrates, nanowires, ultrathin films, or photon detectors adapted
for conducting electricity or acting as batteries, membrane fuel
cells, supercapacitors, superconductors, electromagnetic or
electro-optical actuators, or microelectromechanical devices;
[0138] sheets or structures with variable optical properties;
[0139] sheets adapted for use as heat conductors, heat sinks,
building and reinforcing material, automotive, marine, or aviation
or aerospace panels; [0140] tubular or I-beam cross sectional items
adapted for use as conduits or structural members; and/or [0141] an
electron source adapted for use in: [0142] electron microscopy;
[0143] field emission lighting; [0144] x-ray source; [0145] space
propulsion; [0146] traveling wave tube amplifiers; [0147] air
remediation; [0148] water remediation; or [0149] cold field
emission, etc.
[0150] FIG. 23 is a block diagram of an exemplary embodiment of a
reactor system 23000, which can comprise carbon 23100, a tube
control agent 23200, a catalyst 23300, a transformation process
23400, and an item 23500. Carbon 23100 can be obtained from a
starch, a bean bearing plant, cloth, wood, a plant, and/or a
cellulose or cellulosic product, etc. Carbon 23100 can be partially
obtained from an additive. Tube control agent 23200 can be any tube
control agent described elsewhere herein. Catalyst 23300 can be any
catalyst described elsewhere herein. Item 23500 can be any of, for
example, [0151] components adapted for use as armor or a covering
that at least partially resists penetration by a projectile,
radiation, chemical agents, or biological agents; [0152] adhesive
surfaces; [0153] apparel, footwear, or fabrics adapted for use as a
tarp, weather-resistant covering, or sail; [0154] substrates
adapted for acoustic, infrared, ultraviolet, or other
electromagnetic radiation detection; [0155] substrates adapted to
form tires, railroad bogies, friction control, or vibration control
devices; [0156] load-bearing lines adapted for use in parachutes,
draglines, cargo containers, netting, or connecting lines; [0157]
moorings adapted for land-based, aquatic, aerial, or outer space
applications; [0158] structures adapted for load-bearing or
retention applications in construction, including buildings,
scaffolds, marine vessel hulls, components, or fittings; [0159]
construction materials adapted for use in structures; [0160]
metallic alloys adapted for use in structures, the metallic alloys
comprising nano carbon structures and at least one metal; [0161]
ceramic composites adapted for use in structures, the ceramic
composites comprising nano carbon structures and at least one
ceramic material; [0162] a structure comprising a heat resistant
composite adapted to resist thermal decomposition to at least 1500
degrees Celsius; [0163] superconductor composites adapted for use
in structures, the superconductor composites prepared at
temperature higher than 1500 degrees Celsius, the superconductor
composites comprising nano carbon structures and at least one
superconducting material; [0164] high temperature composites
adapted for use in structures; [0165] aircraft or aerospace
fuselages or structures, or land-based vehicle components,
including body parts, engine components, or brake linings; [0166]
rotation parts adapted for use in at least one of: [0167] vehicles;
[0168] transportation devices, [0169] rotating equipment; or [0170]
rotating tools; [0171] bearings; [0172] composites adapted for use
in paints adapted to resist scratches and wear caused by an impact
or collision; [0173] colorants adapted for use in ceramic
coloration process, processing at high heat condition; [0174]
composites adapted for use in brick; [0175] composites adapted for
use in biomechanical devices; surgical implants; tissue-engineering
structures including bone, tendon, muscle, nerve, skin implants or
surrogates; wound-healing structures, or molecular capture devices
adapted for timed drug delivery; [0176] nano-cantilevers adapted
for biosensing, cell growth, or orthopedic, vascular, or neural
prostheses; [0177] filters, barriers, or wipes; [0178] sheets,
substrates, nanowires, ultrathin films, or photon detectors adapted
for conducting electricity or acting as batteries, membrane fuel
cells, supercapacitors, superconductors, electromagnetic or
electro-optical actuators, or microelectromechanical devices;
[0179] sheets or structures with variable optical properties;
[0180] sheets adapted for use as heat conductors, heat sinks,
building and reinforcing material, automotive, marine, or aviation
or aerospace panels; [0181] tubular or I-beam cross sectional items
adapted for use as conduits or structural members; and/or [0182] an
electron source adapted for use in: [0183] electron microscopy;
[0184] field emission lighting; [0185] x-ray source; [0186] space
propulsion; [0187] traveling wave tube amplifiers; [0188] air
remediation; [0189] water remediation; or [0190] cold field
emission, etc.
[0191] FIG. 24 is a table of thermogravimetric analysis data for
certain exemplary embodiments. FIG. 24 shows TGA data of CNT
synthesized in solid phase using pine wood as a carbon source. All
of MS was substantially completely removed before the TGA test.
Residue mass at approximately 1400.degree. C. was always above 62%,
some reached as high as 81.86%. After an acid wash more that 99%
pure carbon products were achieved. After chemical processing, the
mass loss was less than approximately 5%.
DEFINITIONS
[0192] When the following terms are used substantively herein, the
accompanying definitions apply. These terms and definitions are
presented without prejudice, and, consistent with the application,
the right to redefine these terms during the prosecution of this
application or any application claiming priority hereto is
reserved. For the purpose of interpreting a claim of any patent
that claims priority hereto, each definition (or redefined term if
an original definition was amended during the prosecution of that
patent), functions as a clear and unambiguous disavowal of the
subject matter outside of that definition. [0193] a--at least one.
[0194] activity--an action, act, step, and/or process or portion
thereof. [0195] adapted to--made suitable or fit for a specific use
or situation. [0196] additive--a first substance added to second
substance or product in order to modify one or more properties of
the second substance. [0197] and/or--either in conjunction with or
in alternative to. [0198] animal--a multicellular organism that is
usually mobile, whose cells are not encased in a rigid cell wall
(distinguishing it from plants and fungi) and which derives energy
solely from the consumption of other organisms. [0199]
apparatus--an appliance or device for a particular purpose. [0200]
associate--to join, connect together, and/or relate. [0201] bean--a
relatively large edible seed of plants of several genera of
Fabaceae. [0202] can--is capable of, in at least some embodiments.
[0203] carbon nanotube--a fullerene molecule having a cylindrical
or toroidal shape; the nanotube diameter can range from on the
order of a few nanometers (approximately 1/50,000th of the width of
a human hair) to greater than 18 centimeters in length. [0204]
catalyst--a substance that initiates or accelerates a chemical
reaction without itself being affected by the chemical reaction.
[0205] cause--to produce an effect. [0206] ceramic composite--a
substance comprising a ceramic material that forms a substantially
continuous matrix and at least one other ceramic or non-ceramic
material dispersed in the substantially continuous matrix. [0207]
ceramic material--an inorganic, non-metallic solid prepared by the
action of heat and subsequent cooling; ceramic materials can have a
crystalline or partly crystalline structure, or may be amorphous
(e.g., a glass). [0208] cloth--a woven fabric. [0209] composite--an
engineered material made from two or more constituent materials
with significantly different physical or chemical properties, which
remain separate and distinct on a macroscopic level within the
engineered material structure. [0210] comprising--including but not
limited to. [0211] construction materials--substances adapted for
use in building a device and/or system; construction materials
comprise bricks and metallic frames; construction materials can
comprise alloys of nano carbon and at least one metal. [0212]
convert--to transform, adapt, and/or change. [0213] create--to
bring into being. [0214] define--to establish the outline, form, or
structure of. [0215] determine--to obtain, calculate, decide,
deduce, and/or ascertain. [0216] device--a machine, manufacture,
and/or collection thereof. [0217] fatty acid--any of a class of
aliphatic carboxylic acids, of general formula
C.sub.nH.sub.2n+1COOH, that occur combined with glycerol as animal
or vegetable oils and fats. [0218] generate--to create, produce,
give rise to, and/or bring into existence. [0219] hetero atom--any
atom that is not carbon or hydrogen, such as, nitrogen, oxygen,
sulfur, phosphorus, boron, chlorine, bromine, or iodine. [0220]
high temperature composite--a substance comprising nano carbon
structures and at least one rare earth material, the substance
treated at a temperature higher than 1500 degrees Celsius. [0221]
initialize--to prepare something for use and/or some future event.
[0222] item--an object of a set of objects. [0223] ad-bearing--a
device and/or system adapted to resist deformation from applied
weight. [0224] may--is allowed and/or permitted to, in at least
some embodiments. [0225] metal salt--an ionic compound composed of
a cationic metal (a positively charged ion) and an anion (negative
ion) so that the product is electrically neutral (without a net
charge). [0226] metallic--comprising a metal; a metal is an
element, compound, or alloy characterized by relatively high
electrical conductivity; metals occupy most of the periodic table,
while non-metallic elements can only be found on the
right-hand-side of the Periodic Table of the Elements. A diagonal
line drawn from boron (B) to polonium (Po) separates the metals
from the nonmetals. [0227] method--a process, procedure, and/or
collection of related activities for accomplishing something.
[0228] mooring--a device and/or system adapted to hold secure an
object via cables, anchors, or lines. [0229] nano-cantilever--a
strip of silicon carbide, a few hundred nanometers in width, whose
vibrational frequency varies in proportion to a mass of objects
resting thereon. [0230] oil--any substance that is liquid at
ambient temperatures and is hydrophobic but soluble in organic
solvents. [0231] organometallic compound--a substance comprising a
chemical bond between carbon and a metal. [0232] penetrate--to pass
into or through, such as by overcoming resistance. [0233] plant--an
organism, living or previously living, lacking a capability of
locomotion. [0234] plurality--the state of being plural and/or more
than one. [0235] powder--a dry solid comprising particles having a
diameter that is less than approximately 75 microns. [0236]
provide--to furnish, supply, give, and/or make available. [0237]
receive--to get as a signal, take, acquire, and/or obtain. [0238]
resist--to withstand a force. [0239] select--to make a choice or
selection from alternatives. [0240] set--a related plurality.
[0241] sheet--a substantially planar object that is thin relative
to its length and width. [0242] starch--a carbohydrate consisting
of a large number of glucose units joined together by glycosidic
bonds. [0243] structure--a device and/or system that is constructed
of many distinct parts. [0244] structure formula--a graphical
representation of the molecular structure, of a substance showing
how the atoms are arranged. [0245] substantially--to a great extent
or degree. [0246] substrate--a first stratum or layer lying
underneath a second stratum or layer. [0247] superconductor--a
material having an electrical resistance of approximately zero.
[0248] system--a collection of mechanisms, devices, machines,
articles of manufacture, processes, data, and/or instructions, the
collection designed to perform one or more specific functions.
[0249] tube control agent--a substance adapted to regulate a shape
and/or formation mechanism of a carbon nanostructure. [0250]
via--by way of and/or utilizing. [0251] wood--an organic material,
a natural composite of cellulose fibers (which are strong in
tension) embedded in a matrix of lignin which resists
compression.
Note
[0252] Still other substantially and specifically practical and
useful embodiments will become readily apparent to those skilled in
this art from reading the above-recited and/or herein-included
detailed description and/or drawings of certain exemplary
embodiments. It should be understood that numerous variations,
modifications, and additional embodiments are possible, and
accordingly, all such variations, modifications, and embodiments
are to be regarded as being within the scope of this
application.
[0253] Thus, regardless of the content of any portion (e.g., title,
field, background, summary, description, abstract, drawing figure,
etc.) of this application, unless clearly specified to the
contrary, such as via explicit definition, assertion, or argument,
with respect to any claim, whether of this application and/or any
claim of any application claiming priority hereto, and whether
originally presented or otherwise:
there is no requirement for the inclusion of any particular
described or illustrated characteristic, function; activity, or
element, any particular sequence of activities, or any particular
interrelationship of elements; no characteristic, function,
activity, or element is "essential"; any elements can be
integrated, segregated, and/or duplicated; any activity can be
repeated, any activity can be performed by multiple entities,
and/or any activity can be performed in multiple jurisdictions; and
any activity or element can be specifically excluded, the sequence
of activities can vary, and/or the interrelationship of elements
can vary.
[0254] Moreover, when any number or range is described herein,
unless clearly stated otherwise, that number or range is
approximate. When any range is described herein, unless clearly
stated otherwise, that range includes all values therein and all
subranges therein. For example, if a range of 1 to 10 is described,
that range includes all values therebetween, such as for example,
1.1, 2.5, 3.335, 5, 6.179, 8.9999, etc., and includes all subranges
therebetween, such as for example, 1 to 3.65, 2.8 to 8.14, 1.93 to
9, etc.
[0255] When any claim element is followed by a drawing element
number, that drawing element number is exemplary and non-limiting
on claim scope. No claim of this application is intended to invoke
paragraph six of 35 USC 112 unless the precise phrase "means for"
is followed by a gerund.
[0256] Any information in any material (e.g., a United States
patent, United States patent application, book, article, etc.) that
has been incorporated by reference herein, is only incorporated by
reference to the extent that no conflict exists between such
information and the other statements and drawings set forth herein.
In the event of such conflict, including a conflict that would
render invalid any claim herein or seeking priority hereto, then
any such conflicting information in such material is specifically
not incorporated by reference herein.
[0257] Accordingly, every portion (e.g., title, field, background,
summary, description, abstract, drawing figure, etc.) of this
application, other than the claims themselves, is to be regarded as
illustrative in nature, and not as restrictive, and the scope of
subject matter protected by any patent that issues based on this
application is defined only by the claims of that patent.
* * * * *
References