WO2022154985A1 - Constructions de nanotubes de carbone présentant un gradient de densité et leurs procédés de préparation - Google Patents
Constructions de nanotubes de carbone présentant un gradient de densité et leurs procédés de préparation Download PDFInfo
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- WO2022154985A1 WO2022154985A1 PCT/US2021/072357 US2021072357W WO2022154985A1 WO 2022154985 A1 WO2022154985 A1 WO 2022154985A1 US 2021072357 W US2021072357 W US 2021072357W WO 2022154985 A1 WO2022154985 A1 WO 2022154985A1
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- carbon nanotube
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- construct
- carbon
- carbon nanotubes
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 267
- 239000002041 carbon nanotube Substances 0.000 title claims abstract description 265
- 229910021393 carbon nanotube Inorganic materials 0.000 title claims abstract description 264
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- XTHPWXDJESJLNJ-UHFFFAOYSA-N chlorosulfonic acid Substances OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
Definitions
- the present disclosure relates to carbon nanotubes and constructs formed therefrom.
- Carbon nanotubes are high aspect ratio materials having a variety of mechanical, electrical, and thermal properties that make them attractive for bottom-up construction of aerogels, yams and polymer composites, among other designed structures. Processing of carbon nanotubes has largely focused on spinning carbon nanotubes and bundles thereof into maximal density fibers/yams as a replacement for traditional carbon fibers, such as those used in the formation of polymer composites. However, the potential of carbon nanotubes and their constructs in polymer composites is not fully realized by this carbon fiber replacement approach. In particular, the maximal density structures may reduce the infiltration and integration of polymers. Other advantages to afford improved CNT-matrix interactions include the increased contribution of the interfacial polymer properties to the bulk properties.
- the presence of strongly attractive surfaces can appreciably improve the properties of the polymer molecules in the vicinity of the CNTs.
- the infiltration of polymer may lead to improved stress transfer as the mediating polymer layer is stronger than neat CNT-CNT interfaces.
- the present disclosure is directed to carbon nanotube constructs, including a plurality of first regions including a first plurality of carbon nanotube bundles that are aligned substantially in parallel; a plurality of second regions including a second plurality of carbon nanotube bundles that extend from the plurality of first regions and are non-aligned with the first plurality of carbon nanotube bundles in the plurality of first regions; and an interpenetration region between the plurality of first regions in which the second plurality of carbon nanotubes within second regions extending from one or more adjacent first regions interpenetrate one another.
- the present disclosure is directed to methods that include: providing a plurality of carbon nanotube bundles; and converting the plurality of carbon nanotube bundles into a carbon nanotube construct by applying at least one of stretching force, compression, or elastocapillary coalescence, wherein the carbon nanotube construct includes: a plurality of first regions including a first plurality of carbon nanotubes that are aligned substantially in parallel; a plurality of second regions including a second plurality of carbon nanotubes that extend from the plurality of first regions and are non-aligned with the first plurality of carbon nanotubes in the plurality of first regions; and an interpenetration region between the plurality of first regions in which the second plurality of carbon nanotubes within second regions extending from one or more adjacent first regions interpenetrate one another.
- FIG. 1 is a diagram of a carbon nanotube assembly having tertiary structure.
- FIG. 2 is a cross-sectional diagram of a portion of a carbon nanotube construct of the present disclosure.
- FIGS. 3A and 3B show diagrams of carbon nanotube constructs having additional density variation on the macroscale.
- FIGS. 4 and 5 are plots of specific strength versus specific modulus for carbon nanotube yams and sheets, respectively, produced through various post-processing techniques.
- the present disclosure relates to carbon nanotubes and constructs formed therefrom, including polymer composites that include carbon nanotube constructs having regions of variable carbon nanotube density.
- carbon nanotube constructs disclosed herein include three- dimensional architectures formed from carbon nanotubes as primary structural components.
- regions of variable carbon nanotube density including higher-order carbon nanotube structures having zones with variable density, can be introduced to form complex architectures, as explained further herein.
- Such carbon nanotube constructs may exhibit enhanced mechanical properties and can be processed further to create polymer composites.
- Carbon nanotube constructs are macroscale architectures prepared from micro- and nanoscale assemblies of carbon nanotubes.
- the macroscale architecture of carbon nanotube constructs may also include regions of variable density created through interpenetration of neighboring microscale carbon nanotube assemblies that define the construct.
- the regions of variable density may enhance the impregnation with polymeric materials (polymer matrices or polymer resins), wetting, and improved space filling, particularly when compared to densely organized carbon materials, such as well-packed carbon nanotube yams.
- carbon nanotube constructs can exhibit progressive failure modes in which the architecture can sustain increased amounts of carbon nanotube damage prior to catastrophic failure, in contrast to the sudden failure and elastic recoil (ballistic failure) observed in dense carbon fiber-based structures.
- Structural redundancy and enhanced stress transmission throughout the interpenetrating networks within a carbon nanotube construct can allow stored strain energy to dissipate gradually, reducing ballistic failure and further damage progression to neighboring zones of the carbon nanotube construct and/or the surrounding polymer matrix.
- Carbon nanotubes represent the primary structural component (building block) of the carbon nanotube constructs.
- “carbon nanotubes” are diverse carbon-based structures that may include single-wall carbon nanotubes, multi-wall carbon nanotubes, double-wall carbon nanotubes, few-wall carbon nanotubes, and mixtures thereof.
- carbon nanotubes can be separated and/or enriched based on particular properties such as chirality, electrical conductivity, thermal conductivity, diameter, length, number of walls, defect density, and any combination of these properties.
- Suitable carbon nanotubes can have a ratio of diameter to length (aspect ratio) of at least about 10 3 , which can be an aspect ratio in a range of about 10 3 to about 10 8 in some embodiments. While carbon nanotube lengths may vary according to synthesis methods, suitable carbon nanotubes may have a length of at least about 100 microns in some embodiments.
- Carbon nanotube constructs disclosed herein can also be formed in whole or in part from carbon nanotubes functionalized with various surface modifications and substitutions.
- Functionalization may be employed, for example, to attenuate or enhance intermolecular van der Waals forces and enhance affinity with solvents, polymers, and/or polymer resins.
- Functionalization can also include various crosslinking chemistries that facilitate covalent and non-covalent linking between carbon nanotubes and/or polymer matrix for improved material properties and stress transfer.
- a wide range of techniques for functionalizing carbon nanotubes and functional groups introduced thereto will be familiar to one having ordinary skill in the art.
- secondary structures may develop from linear networks of carbon nanotubes oriented in a parallel or near- parallel fashion.
- Such linear networks of carbon nanotubes may be referred to as “carbon nanotube bundles” and can have diameters that range from about 30 nm or more, such as within a range of 20 nm to 75 nm or 30 nm to 50 nm, depending on the method of synthesis.
- Carbon nanotube bundles may be obtained, for example, by floating catalyst chemical vapor deposition (FCCVD), followed by various post-processing methods.
- Carbon nanotubes generated by FCCVD may include carbon nanotubes of various lengths up to about 1 mm or more, which can be processed to form low-density aerogels and/or incorporated into polymer composites using processes analogous to those used for comparatively high-density carbon fibers.
- FCCVD synthesis methods can also be adapted for continuous collection and processing. While carbon nanotubes prepared by FCCVD may be particularly suitable in the disclosure herein, the principles of the present disclosure are also applicable to carbon nanotubes produced by other techniques such as arc discharge, laser oven, flame synthesis, chemical vapor deposition, and the like.
- Carbon nanotube bundles can interface to form larger tertiary structures (or “carbon nanotube assemblies”) that include interpenetrating networks of carbon nanotubes, including “bristly” carbon nanotube assemblies containing three-dimensional mixtures containing subpopulations of both substantially parallel- and substantially non-parallel-oriented carbon nanotube bundles.
- “Substantially non-parallel-oriented” carbon nanotube bundles include any carbon nanotube bundle orientation that is not oriented substantially parallel with respect to another carbon nanotube bundle, particularly a plurality of carbon nanotube bundles aligned substantially in parallel, and is inclusive of carbon nanotube bundles oriented perpendicular to another carbon nanotube bundle and carbon nanotube bundles that are oriented irregularly with respect to another carbon nanotube bundle (any non-perpendicular angle except for parallel alignment).
- At least a majority of the carbon nanotube bundles arranged in a non-aligned fashion with parallel- aligned carbon nanotube bundles are arranged in a non-perpendicular fashion with respect to the parallel-aligned carbon nanotube bundles, more preferably in an irregular fashion with respect to the parallel-aligned carbon nanotube bundles.
- a plurality of non-aligned carbon nanotubes bundles may be oriented at a plurality of non-perpendicular angles in the constructs disclosed herein.
- Carbon nanotube construct 300b in FIG. 3B has spatially distributed density in two dimensions with high-density zones 302 and low-density zones 304. While shown in a checkerboard pattern in FIG. 3B, it is to be appreciated that other regular spatial arrangements for high-density zones 302 and low-density zones 304 also reside within the scope of the present disclosure. Likewise, irregular arrangements of high-density zones 302 and low-density zones 304 in two-dimensional constructs also reside within the scope of the present disclosure. High- density zones 302 and low-density zones 304 can be produced by various post-processing methods described below.
- Post-processing methods can also combine techniques, including extensional stretching and/or compression in the presence of at least one of a solvent, polymer solution containing monomers, prepolymers, and/or polymers, or an acid.
- acid treatment can be combined with extensional stretching, which may improve debundling by solvation and removal of byproducts.
- Post-processing techniques may also include covalently crosslinking the carbon nanotubes within a carbon nanotube construct to enhance stress transfer throughout the carbon nanotube network.
- Illustrative crosslinking techniques may include for example, irradiation by e- beam, plasma, gamma radiation, and the like, and/or by the use of crosslinking chemistry.
- Element 3 wherein the plurality of second regions have a local density in a range of about 0.5 g/cm 3 to about 1.0 g/cm 3 .
- Element 12 wherein the carbon nanotube construct is a yam.
- Element 14 wherein the polymer matrix is present within at least the interpenetration region and/or the plurality of second regions.
- Embodiment B further including: generating a three-dimensional shape from the carbon nanotube construct by a laying up process.
- Element 19 wherein the plurality of second regions have a local density in a range of about 0.5 g/cm 3 to about 1.0 g/cm 3 .
- Element 20 wherein converting comprises applying tension to the carbon nanotube bundles.
- illustrative combinations applicable to A include, but are not limited to, A and Element 1, A and Element 2, A and Element 3, A and Element 4, A and Element 5, A and Element 6, A and Element 7, A and Element 8, A and Element 9, A and Element 10, A and Element 11, A and Element 12, A and Element 13, A and Element 14, A and Element 15, and A and Element 16.
- Illustrative combinations applicable to B include, but are not limited to, B and Element 17, B and Element 18, B and Element 19, B and Element 20, and B and Element 2E
- compositions described herein may be free of any component, or composition not expressly recited or disclosed herein. Any method may lack any step not recited or disclosed herein.
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
L'invention concerne des constructions de nanotubes de carbone qui peuvent comprendre une pluralité de premières régions comprenant une première pluralité de groupes de nanotubes de carbone qui sont alignés sensiblement de manière parallèle; une pluralité de secondes régions comprenant une seconde pluralité de groupes de nanotubes de carbone qui s'étendent à partir de la pluralité de premières régions et qui ne sont pas alignés avec la première pluralité de groupes de nanotubes de carbone dans la pluralité de premières régions; et une région d'interpénétration entre la pluralité de premières régions dans laquelle la seconde pluralité de nanotubes de carbone dans des secondes régions s'étendant depuis une ou plusieurs premières régions adjacentes s'interpénètrent les unes dans les autres. Les procédés peuvent consister à fournir une pluralité de groupes de nanotubes de carbone; et à convertir la pluralité de groupes de nanotubes de carbone en une construction de nanotubes de carbone par application d'une force d'étirage, et/ou d'une compression, et/ou d'une coalescence élastocapillaire.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US202163136661P | 2021-01-13 | 2021-01-13 | |
| US63/136,661 | 2021-01-13 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2022154985A1 true WO2022154985A1 (fr) | 2022-07-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/US2021/072357 WO2022154985A1 (fr) | 2021-01-13 | 2021-11-11 | Constructions de nanotubes de carbone présentant un gradient de densité et leurs procédés de préparation |
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| Country | Link |
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| WO (1) | WO2022154985A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210323826A1 (en) * | 2020-04-17 | 2021-10-21 | Korea Institute Of Science And Technology | Method for producing densified carbon nanotube fiber |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030165648A1 (en) * | 2002-03-04 | 2003-09-04 | Alex Lobovsky | Composite material comprising oriented carbon nanotubes in a carbon matrix and process for preparing same |
| US7045108B2 (en) * | 2002-09-16 | 2006-05-16 | Tsinghua University | Method for fabricating carbon nanotube yarn |
| WO2007008214A1 (fr) * | 2004-07-22 | 2007-01-18 | William Marsh Rice University | Reseaux imbriques de polymere/nanotube de carbone et procede de fabrication correspondant |
| WO2007015710A2 (fr) * | 2004-11-09 | 2007-02-08 | Board Of Regents, The University Of Texas System | Fabrication et applications de rubans, feuilles et fils retors ou non de nanofibres |
-
2021
- 2021-11-11 WO PCT/US2021/072357 patent/WO2022154985A1/fr active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030165648A1 (en) * | 2002-03-04 | 2003-09-04 | Alex Lobovsky | Composite material comprising oriented carbon nanotubes in a carbon matrix and process for preparing same |
| US7045108B2 (en) * | 2002-09-16 | 2006-05-16 | Tsinghua University | Method for fabricating carbon nanotube yarn |
| WO2007008214A1 (fr) * | 2004-07-22 | 2007-01-18 | William Marsh Rice University | Reseaux imbriques de polymere/nanotube de carbone et procede de fabrication correspondant |
| WO2007015710A2 (fr) * | 2004-11-09 | 2007-02-08 | Board Of Regents, The University Of Texas System | Fabrication et applications de rubans, feuilles et fils retors ou non de nanofibres |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20210323826A1 (en) * | 2020-04-17 | 2021-10-21 | Korea Institute Of Science And Technology | Method for producing densified carbon nanotube fiber |
| US11897770B2 (en) * | 2020-04-17 | 2024-02-13 | Korea Institute Of Science And Technology | Method for producing densified carbon nanotube fiber |
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