WO2013133941A1 - Carbon nanotube reinforced nanocomposites - Google Patents
Carbon nanotube reinforced nanocomposites Download PDFInfo
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- WO2013133941A1 WO2013133941A1 PCT/US2013/025866 US2013025866W WO2013133941A1 WO 2013133941 A1 WO2013133941 A1 WO 2013133941A1 US 2013025866 W US2013025866 W US 2013025866W WO 2013133941 A1 WO2013133941 A1 WO 2013133941A1
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- Prior art keywords
- carbon nanotubes
- walled carbon
- composite
- recited
- walled
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- 239000002041 carbon nanotube Substances 0.000 title claims description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims description 33
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims description 22
- 239000002114 nanocomposite Substances 0.000 title abstract description 23
- 239000004593 Epoxy Substances 0.000 claims abstract description 52
- 239000002048 multi walled nanotube Substances 0.000 claims abstract description 38
- 239000002109 single walled nanotube Substances 0.000 claims abstract description 36
- 229920001187 thermosetting polymer Polymers 0.000 claims abstract description 10
- 239000002079 double walled nanotube Substances 0.000 claims abstract 9
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract 8
- 238000000034 method Methods 0.000 claims description 19
- 229910052799 carbon Inorganic materials 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims 31
- 239000002071 nanotube Substances 0.000 claims 4
- 229920000642 polymer Polymers 0.000 abstract description 6
- 238000011068 loading method Methods 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- 230000002787 reinforcement Effects 0.000 description 6
- 239000011159 matrix material Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 3
- 239000004848 polyfunctional curative Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- -1 DWNTs Substances 0.000 description 1
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000004643 cyanate ester Substances 0.000 description 1
- 150000001913 cyanates Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
- 229920006305 unsaturated polyester Polymers 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Definitions
- FIG. 1 illustrates a process for .manufacturing epoxy/carbon nanotube (“CNT”) nanocomposites in accordance with embodiments of the present invention-
- a combination of multi-walled carbon rianotubes (“MWNTs”) (herein, MWNTs have more than two wails) and double-walled CNTs (“DWNTs”) significantly improves the mechanical properties of polymer nanocomposites,
- MWNTs multi-walled carbon rianotubes
- DWNTs double-walled CNTs
- a small amount of DWNTs reinforcement e.g., ⁇ 1 wt,%) significantly improves the flexural strength of epoxy matri nanocomposiles.
- a same or similar amount of MWNTs reinforcement significantly improves the .flexural modulus (stiffness) of epoxy matrix . nanocomposites.
- Both flexural strength and flexural modulus of the .MWNTs and DWNTs co-reinforced epoxy nanocomposites are further improved compared with same amount of either DWNTs or MWNTs reinforced epoxy nanoeoniposit.es.
- Besides epoxy, other thetinoset pctlymers may also be utilized.
- SWNTs single-walled CNTs
- MWNTs MWNTs
- SWNTs MWNTs
- a small amount of SWNTs reinforcement e.g., ⁇ 1 wt.% significantly improves the flexural strength of epoxy matrix nanocomposites.
- a same or similar amount of MWNTs reinforcement significantly improves the flexural modulus (stiffness) of epoxy matrix, nanocomposites.
- a combination of MWNTs and SWNTs and DWNTs also significantly improves the mechanical properties of polymer .nanocomposites.
- a small amount of SWNTs/DWNTs reinforcement e.g., ⁇ 1 wt.%) significantly improves the ilexural strength of epoxy matrix nanocoinposites.
- a same or similar amount of MWNTs reinforcement significantly improves the ilexural modulus (stiffness ⁇ of epoxy matrix nanocomposites.
- Both ilexural strength and ilexural modulus of the MWNTs aud SWNTs and DWNTs co- reinforced epoxy nanocomposites are fi.wth.er improved compared with same amount of either SWNTs or DWNTs or MWNTs reinforced epoxy nanocomposites.
- other thermoxet polymers may also work.
- MWNTs, SWNTs, and DWNTs are also simply referred to as CNTs herein when discussed in a more general sense.
- Epoxy resin hisphenol-A
- a hardener dicyandiamide
- the hardener was used to cure the epoxy nanocomposites.
- SWNTs, DWNTs, and MWNTs were commercially obtained.
- the CNTs may be funciionaiized with amino ⁇ NI3 ⁇ 4) Junctional groups. Amino-funetiona!ized CNTs may help to improve the bonding between the CNTs and epoxy molecular chairs, which can further improve the mechanical properties of the nanocomposites.
- pristine CNTs or tuncttonalfeed by other means may also work.
- Thermosetting polymers that may be used as described herein include, but are not limited to, epoxies, vinyl esters, unsaturated polyesters, phenolics, cyanate esters (CBs), bismaieimides (BMls), polyimides, or any combination thereof
- FIG. I illustrates a schematic diagram of a process flow to make epoxy/CNT nanocomposites. All ingredients may be dried (e.g., in a vacuum oven at approximately 70°C for approximately 16 hours ⁇ to remove moisture, in step 101, the CNTs were placed in a solvent (e.g., acetone) and dispersed (e.g., by a micro-iliiidie machine commercially available from Microtluidics Co.) in step 102.
- the micro-fluidic machine uses high- pressure streams that collide at. uUra-high velocities in precisely defined micron-sized channels. Its combined forces of shear and impact act upon products to create uniform dispersions.
- the CNT solution was then formed as a gel in step 103 resulting in the CNTs well dispersed in the solution.
- other methods such as an ultrasonieation process, may also be utilized to disperse the CNTs in a solvent.
- a surfactant may be also used t disperse the CNTs in solution.
- Epoxy was then added in step 104 to the CNT/solvent gel to create an epoxy/CNT/solvent solution 105, which was followed by another mixing process 106 (e.g., u!trasonication in a bath at approximately 70°C for approximately 1 hour) to create an epoxy/CNT/solvent suspension 107,
- the CNTs were further dispersed in epoxy in step 108 (e.g., using a stirrer mixing process at approximately 70 C C for approximately half an hour at a speed of approximately 1,400 rev/min. to create an. epoxy/CNT/solvent ge!. 109.
- a hardener was than added in step 1 10 to the epoxy/CNT/solvent gel.
- step 1 109 e.g., at a ratio of approximately 4.5 wt.% followed by stirring (e.g., at approximately 70°C for approximately 1 hour ⁇ .
- I l l was degassed in step 1 1.2 (e.g., in a vacuum oven at approximately ?0°C tor approximately 48 hours).
- the material 1 13 was then poured into a mold (e.g.. Teflon) and cured (e.g., at approximately 160*C for approximately 2 hours).
- Mechanical properties (flexurai strength and fiexural modulus) of the specimens were characterized in step 1 .15 after an optional polishing process.
- Table 1 shows the mechanical, properties (tlexural strength and flexurai. modulus) of the epoxies made using the process flow of FIG. 1 to make epoxy/CNT nanocomposites.
- the fiexural strength of epoxy/DWNTs is higher than that of epoxy MW Ts at the same loading of CNTs, while the fiexural modulus of epoxy/DWNTs is lower than that of epoxy/MWNTs at the same loading of CNTs.
- Both the fiexural. strength and flexurai modulus of epoxy/DWNTs are higher than those of epoxy/DWNTs (1 wt.%),
- the flexurai strength of epoxy/SWNTs is higher than that of epoxy/MWNTs at. the same loading of CNTs, white the flexurai modulus of epoxy/SWNTs is lower than that of epoxyMWNTs at the same loading of CNTs.
- Both the fiexural strength and fiexural modulus of epoxy/SWNTs (0.5 wt.%)/ WNTs (0.5 wt.%) are higher than those of epoxy/SWNTs (.1 wt.%).
Abstract
A combination of multi-walled carbon nanotubes and single-walled carbon nanotubes and/or double-walled carbon nanotubes significantly improves the mechanical properties of polymer nanocomposites. Both flexural strength and flexural modulus of the MWNTs and single-walled carbon nanotubes and/or double-walled carbon nanotubes co-reinforced epoxy nanocomposites are further improved compared with same amount of either single-walled carbon nanotubes and/or double-walled carbon nanotubes or multi-walled carbon nanotubes reinforced epoxy nanocomposites. Besides epoxy, other thermoset polymers may also work.
Description
Carbon Nanotu.be Reinforced. Nanocomposites
This application is a continuation-in-part application of U.S. Patent Application Serial No. 1 1/693,454, issued as U.S. Patent No, 8,1.29,463, which claims priority to U.S. Provisional Application Serial Nos, 60/788,234 and 60/810,394, ail of which are hereby incorporated, by reference herein.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 illustrates a process for .manufacturing epoxy/carbon nanotube ("CNT") nanocomposites in accordance with embodiments of the present invention-
DETAILED DESCRIPTIO
A combination of multi-walled carbon rianotubes ("MWNTs") (herein, MWNTs have more than two wails) and double-walled CNTs ("DWNTs") significantly improves the mechanical properties of polymer nanocomposites, A small amount of DWNTs reinforcement (e.g., <1 wt,%) significantly improves the flexural strength of epoxy matri nanocomposiles. A same or similar amount of MWNTs reinforcement significantly improves the .flexural modulus (stiffness) of epoxy matrix . nanocomposites. Both flexural strength and flexural modulus of the .MWNTs and DWNTs co-reinforced epoxy nanocomposites are further improved compared with same amount of either DWNTs or MWNTs reinforced epoxy nanoeoniposit.es. Besides epoxy, other thetinoset pctlymers may also be utilized.
In this nanocomposite system, single-walled CNTs ("SWNTs") may also work instead of DWNTs. Therefore, a combination of MWNTs and. SWNTs also significantly improves the mechaniea! properties of polymer nanocomposites. A small amount of SWNTs reinforcement (e.g., <1 wt.%) significantly improves the flexural strength of epoxy matrix nanocomposites. A same or similar amount of MWNTs reinforcement significantly improves the flexural modulus (stiffness) of epoxy matrix, nanocomposites. Both flexural strength and flexural modulus of the MWNTs and SWNTs co-rein forced epoxy nanocomposites are further improved compared with same amount of either SWNTs or MWNTs reinforced epoxy nanocomposites. Besides epoxy, other thermosei polymers may also work.
Furthermore, a combination of MWNTs and SWNTs and DWNTs also significantly improves the mechanical properties of polymer .nanocomposites, A small amount of
SWNTs/DWNTs reinforcement (e.g., <1 wt.%) significantly improves the ilexural strength of epoxy matrix nanocoinposites. A same or similar amount of MWNTs reinforcement significantly improves the ilexural modulus (stiffness} of epoxy matrix nanocomposites. Both ilexural strength and ilexural modulus of the MWNTs aud SWNTs and DWNTs co- reinforced epoxy nanocomposites are fi.wth.er improved compared with same amount of either SWNTs or DWNTs or MWNTs reinforced epoxy nanocomposites. Besides epoxy, other thermoxet polymers may also work.
In embodiments of the present invention, an example is provided. MWNTs, SWNTs, and DWNTs are also simply referred to as CNTs herein when discussed in a more general sense.
Epoxy resin (hisphenol-A) and a hardener (dicyandiamide) was commercially obtained. The hardener was used to cure the epoxy nanocomposites. SWNTs, DWNTs, and MWNTs were commercially obtained. The CNTs may be funciionaiized with amino {~NI¾) Junctional groups. Amino-funetiona!ized CNTs may help to improve the bonding between the CNTs and epoxy molecular chairs, which can further improve the mechanical properties of the nanocomposites. However, pristine CNTs or tuncttonalfeed by other means (such as earboxylk functional groups) may also work. Although epoxy was used as an example for the experimentation, other ihermosets may a!so work. Thermosetting polymers that may be used as described herein include, but are not limited to, epoxies, vinyl esters, unsaturated polyesters, phenolics, cyanate esters (CBs), bismaieimides (BMls), polyimides, or any combination thereof
FIG. I illustrates a schematic diagram of a process flow to make epoxy/CNT nanocomposites. All ingredients may be dried (e.g., in a vacuum oven at approximately 70°C for approximately 16 hours} to remove moisture, in step 101, the CNTs were placed in a solvent (e.g., acetone) and dispersed (e.g., by a micro-iliiidie machine commercially available from Microtluidics Co.) in step 102. The micro-fluidic machine uses high- pressure streams that collide at. uUra-high velocities in precisely defined micron-sized channels. Its combined forces of shear and impact act upon products to create uniform dispersions. The CNT solution was then formed as a gel in step 103 resulting in the CNTs well dispersed in the solution. However, other methods, such as an ultrasonieation process, may also be utilized to disperse the CNTs in a solvent. A surfactant may be also used t disperse the CNTs in solution. Epoxy was then added in step 104 to the CNT/solvent gel to create an epoxy/CNT/solvent solution 105, which was followed by another mixing process
106 (e.g., u!trasonication in a bath at approximately 70°C for approximately 1 hour) to create an epoxy/CNT/solvent suspension 107, The CNTs were further dispersed in epoxy in step 108 (e.g., using a stirrer mixing process at approximately 70CC for approximately half an hour at a speed of approximately 1,400 rev/min. to create an. epoxy/CNT/solvent ge!. 109. A hardener was than added in step 1 10 to the epoxy/CNT/solvent gel. 109 (e.g., at a ratio of approximately 4.5 wt.%) followed by stirring (e.g., at approximately 70°C for approximately 1 hour}. The resulting gel. I l l was degassed in step 1 1.2 (e.g., in a vacuum oven at approximately ?0°C tor approximately 48 hours). The material 1 13 was then poured into a mold (e.g.. Teflon) and cured (e.g., at approximately 160*C for approximately 2 hours). Mechanical properties (flexurai strength and fiexural modulus) of the specimens were characterized in step 1 .15 after an optional polishing process.
Table 1 shows the mechanical, properties (tlexural strength and flexurai. modulus) of the epoxies made using the process flow of FIG. 1 to make epoxy/CNT nanocomposites.
As indicated in Table 3 , the fiexural strength of epoxy/DWNTs is higher than that of epoxy MW Ts at the same loading of CNTs, while the fiexural modulus of epoxy/DWNTs is lower than that of epoxy/MWNTs at the same loading of CNTs. Both the fiexural. strength and flexurai modulus of epoxy/DWNTs (0.5 wt.%) MWNTs (0.5 wt.%) are higher than those of epoxy/DWNTs (1 wt.%),
Also as indicated in Table 1 , the flexurai strength of epoxy/SWNTs is higher than that of epoxy/MWNTs at. the same loading of CNTs, white the flexurai modulus of epoxy/SWNTs is lower than that of epoxyMWNTs at the same loading of CNTs. Both the fiexural strength and fiexural modulus of epoxy/SWNTs (0.5 wt.%)/ WNTs (0.5 wt.%) are higher than those of epoxy/SWNTs (.1 wt.%).
Furthermore as indicated in Table L the fiexural strength of epoxy/SWNT TJWNTs i higher than tha of epoxy/MWNTs at the same loading of CNTs, while the fiexural modulus of epoxy/SWNTs DWNTs is Sower than that of epoxy/MWNTs at the same loading of CNTs. Both the fiexural strength and fiexural modulus of epoxy/SWNTs (0. S wi.%)/DWNTs (0.5 wt.%)/MWNTs (0.5 wt.%) are higher than those of epoxy/SWNTs/DWNTs ( 1 wt.%). Higher loadings of the CNTs ma als work.
Table 1
Claims
1. A composite material comprising:
a thermoset;
single- walled carbon nanotubes; and
multi-walled carbon nanotubes, wherein a total concentration of the carbon nanotubes includes a concentration of the single-walled carbon nanotubes and a concentration of the multi-walled -carbon nanotubes selected such that the composite material has a ilexural strength and a ilexural modulus thai exceed the fiexural strength and the ilexural modulus, respectively, of a composite material comprising the thermoset and substantially a same total concentration of either single-walled carbon nanotiibes or imilti -wailed carbon nanotiibes.
2. The material as recited in claim 1 , wherein the concentrations of the single-walled carbon nanotubes and the multi-walled carbon nanotubes are optimal for increasing both the ilexural strength and the ilexural modulus of the composite material.
3. The material as recited in claim 2, wherein the concentration of the single-walled carbon nanotubes is between 0.01-40 wt.%.
4. The material as recited in claim 2, wherein the concentration of the single-walled carbon nanotubes is between 0.01-20 wt.%,
5. A composite comprising a content of thermoset of 60--99.98 wt.%, a content of multi-walled carbon nanotubes of 0.01-20 wt.%, and a content of single-walled carbon nanotubes of 0. 1-20 wt.%.
6. The composi te of claim 5, wherein the 'thermoset comprises an epoxy.
7. A method for making a carbon nanotube composite by varying an amount of carbon nanotubes to be added to the composite as a function of the diameters of the carbon
nano tubes to increase the ilexural strength and the flex ral modulus of the carbon nanotube composite.
8. The method as recited in claim 7, wherein the carbon nanotubes are single-walled carbon nanotubes.
9. The method as recited in claim 7, wherein the carbon nanotubes are multi-walled carbon, nanotubes.
10. The method as recited in claim 7, wherein a ratio of single-walled carbon nanotubes to multi-walled carbon nanotubes within the composite is varied to increase the flexural strength and the ilexural modulus of the carbon nanoiiibe composite.
1 1. The method as recited in claim 10, wherein, the composite further comprises a thermoset,
12. The method as recited in claim 10, wherein the composite further comprises an epo y.
13. A composite material comprising:
a thermoset;
single-walled carbon nanotubes.
doubie- a!led carbon, nanotubes: and
multi-walled carbon nanotubes, wherein a total concentration of the carbon nanotubes includes a concentration of the single-walled carbon nanotubes, a concentration of the double- walled carbon nanotubes, and a concentration of the multi-walled carbon nanotubes selected such thai the composite material has a ilexural strength and. a ilexural modulus that exceed the ilexural strength and the ilexural modulus, respectively, of a composite material comprising the thermoset and substantially a same total concentration of either single-wailed carbon nanotubes, double- walled carbon .nanotubes, or multi- walled carbon nanotubes,
14. The .material a recited in claim 13, wherein the concentrations of the single- walled carbon nanotubes, the double-wailed carbon nanotubes, and the multi-walled carbon
nanotubes are optimal for increasing both the flexural strengih and the flexural modulus of the composite material
15. The material as recited in claim 1.4, wherein the concentration of the sing!e-walied carbon nanotubes or the double-walled carbon nanotubes is between 0.01-40 wt.%.
16. The material as recited in claim 15, wherein the concentration of the single- walled carbon nanotubes or the double- walled carbo nanotubes is between 0,01-20 wt.%.
17. A composite comprising a content of therraoset of 60-99.98 wt.%, a content of multi-walled carbon nanotubes of 0.01-20 wt.%, a content of double-walled carbon nanotubes of 0,01-20 wt.%, and a content of single-walled carbon nanotubes of 0.01-20 wt.%.
18. The composite of claim I?, wherein the the moset comprises an epoxy.
1 . A method for making a carbon nanotube composite by varying an amount, of carbon nanotubes to be added to the composite as a function of the diameters of the carbon nanotubes to increase the flexural strength and the flexural modulus of the carbon nanotube composite, wherein the carbon nanotubes comprise single-walled carbon nanotubes, double-walled carbon nanotubes, and multi-walled carbon nanotubes.
20. The method as recited in claim 1 , wherein a ratio of single- wal led carbon nanotubes to multi-walled carbon nanotubes within the composite is varied to increase the .flexural strength, and the flexural modulus of the carbon nanotube composite.
21. The method as reci ted in claim 20, wherein a ratio of double-walled carbon nanotubes to multi-walled carbon nanotubes within the composite is varied to increase the flexural strengih and the flexural modulus of the carbon nanotube composite.
.
22. The method as recited in claim 21, wherein a ratio of double-walled carbon nanotube to multi-walled carbon nanotubes within the composite is varied to increase the flexural strength and the flexural modulus of the carbon nanotube composite.
23. The meihod as recited in claim 1 , wherein a ratio of single- walled carbon nanotu es to double- walled carbon nanombes within the composite is varied to increase the ilexiirai strength and the ilexura! modulus of the carbon nanotube composite.
24. The method as recited in claim 19, wherein the composite further comprises a thermoset,
25. The method as recited in claim 19, wherein the composite further comprises an epoxy.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US13/413,633 | 2012-03-06 | ||
| US13/413,633 US20120220695A1 (en) | 2006-03-31 | 2012-03-06 | Carbon Nanotube Reinforced Nanocomposites |
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| WO2013133941A1 true WO2013133941A1 (en) | 2013-09-12 |
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| TWI783231B (en) * | 2019-05-31 | 2022-11-11 | 美商美國琳得科股份有限公司 | Films of multiwall, few wall, and single wall carbon nanotube mixtures |
| US11820659B2 (en) | 2019-05-31 | 2023-11-21 | Lintec Of America, Inc. | Films of multiwall, few wall, and single wall carbon nanotube mixtures |
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