# US 11,111,146 B2 · Carbon nanotube product manufacturing system and method of manufacture thereof

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- Number: US 11,111,146 B2
- Document ID: US11111146B2
- Status: Granted
- Kind: B2
- Application number: 16/152,246
- Filed: 2018-10-04
- Published: 2020-04-09
- Granted: 2021-09-07
- Earliest claimed: 2018-10-04
- Assignees: Wootz, Inc.
- Applicants: Wootz, LLC
- Inventors: Elie Amram Bengio; Alexander Joseph Marks
- Web page: https://patentgrep.com/patent/US11111146B2

## CPC

- C01B 32/174: Derivatisation; Solubilisation; Dispersion in solvents
- B29C 48/0018: {combined with shaping by orienting, stretching or shrinking, e.g. film blowing (B29C48/0017 takes precedence)}
- B29C 48/022: {characterised by the choice of material}
- B29C 48/05: Filamentary, e.g. strands
- B29C 48/88: Thermal treatment of the stream of extruded material, e.g. cooling
- B29C 48/91: Heating, e.g. for cross linking
- D01D 5/06: Wet spinning methods {(D01D5/0046 takes precedence)}
- D01F 1/10: Other agents for modifying properties
- D01F 9/12: Carbon filaments; Apparatus specially adapted for the manufacture thereof
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01B 2202/08: Aligned nanotubes
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B29C: SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING (making preforms B29B11/00; making laminated products by combining previously unconnected layers which become one product whose layers will remain together B32B37/00 - B32B41/00)
- D01D: MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01F: CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

A method of manufacturing a carbon nanotube product comprising: blending an unaligned carbon nanotube material with solid solvent particles; activating a nanotube solvent by liquefying the solid solvent particles; producing a nanotube dope solution by mixing the nanotube solvent and the unaligned carbon nanotube material; forming a carbon nanotube proto-product by extruding the nanotube dope solution; and forming an aligned carbon nanotube product by solidifying the carbon nanotube proto-product.

## Claims

### Claim 1

A method of manufacturing a carbon nanotube product, the method comprising:
blending an unaligned carbon nanotube material comprising carbon nanotube molecules with solid solvent particles;
activating a nanotube solvent by liquefying the solid solvent particles;
producing a nanotube dope solution by mixing the nanotube solvent and the unaligned carbon nanotube material;
forming a carbon nanotube proto-product by extruding the nanotube dope solution, thereby imparting alignment to carbon nanotube molecules of the carbon nanotube proto-product; and
forming an aligned carbon nanotube product by solidifying the carbon nanotube proto-product by:
exposing the carbon nanotube proto-product to an infrared radiation source at a wavelength selected in the range of 1 μm to 130 μm to reduce absorption of the radiation by the nanotube solvent relative to absorption of the radiation by carbon nanotubes of the carbon nanotube proto-product, and
exposing the carbon nanotube proto-product to a chemical coagulant, wherein the chemical coagulant is a solvent for the nanotube solvent and a non-solvent for the carbon nanotube proto-product.

### Claim 2 (depends on 1)

The method of claim 1, wherein forming the carbon nanotube proto-product includes extruding the nanotube dope solution as a nanotube filament.

### Claim 3 (depends on 1)

The method of claim 1, wherein forming the carbon nanotube proto-product includes extruding the nanotube dope solution as a nanotube film.

### Claim 4 (depends on 1)

The method of claim 1, further comprising cryogenically freezing the nanotube solvent to form the solid solvent particles prior to blending with the unaligned carbon nanotube material.

### Claim 5 (depends on 1)

The method of claim 1, wherein activating the nanotube solvent includes heating the solid solvent particles.

### Claim 6 (depends on 1)

The method of claim 1, wherein the nanotube solvent is chlorosulfonic acid.

### Claim 7 (depends on 1)

The method of claim 1, further comprising, prior to extruding the nanotube dope solution, adding an additional amount of the nanotube solvent in a liquid state to the nanotube dope solution.

### Claim 8 (depends on 1)

The method of claim 1, further comprising removing an amount of the nanotube solvent from the nanotube dope solution through evaporation under co-flow with gaseous hydrochloric acid to prevent degradation of the nanotube solvent.

### Claim 9 (depends on 1)

The method of claim 1, wherein producing the nanotube dope solution includes producing the nanotube dope solution at a concentration between 2% and 20% by weight of the unaligned carbon nanotube material.

### Claim 10 (depends on 1)

The method of claim 1, further comprising fractionating the nanotube dope solution to remove carbon nanotube molecules of the lowest aspect ratio from the nanotube dope solution.

### Claim 11 (depends on 1)

The method of claim 1, further comprising drawing the carbon nanotube proto-product to impart further alignment of carbon nanotube molecules in the carbon nanotube proto-product.

### Claim 12 (depends on 1)

The method of claim 1, further comprising thermally annealing the aligned carbon nanotube product to remove an amount of the chemical coagulant from the aligned carbon nanotube product.

### Claim 13 (depends on 1)

The method of claim 1, further comprising doping the aligned carbon nanotube product.

### Claim 14 (depends on 1)

The method of claim 1, further comprising coating the surface of the aligned carbon nanotube product.

### Claim 15 (depends on 1)

The method of claim 1, further comprising integrating the aligned carbon nanotube product with additional instances of the aligned carbon nanotube product, other materials, or a combination thereof, to produce an integrated structure selected from yarns, threads, woven fabrics, laminated films, tape, foam, composite pre-impregnated materials, and discrete length chopped fiber material.

### Claim 16 (depends on 1)

The method of claim 1, further comprising integrating the aligned carbon nanotube product with additional instances of the aligned carbon nanotube product, other materials, or a combination thereof, to produce a component select from wire antennas, patch antennas, coil transformers, and coaxial cables.

### Claim 17 (depends on 1)

The method of claim 1, wherein the infrared radiation is pulsed.

### Claim 18 (depends on 1)

The method of claim 1, wherein forming the aligned carbon nanotube product includes, prior to exposing the carbon nanotube-proto-product to the infrared radiation source, an initial alignment step imposing further alignment on carbon nanotube molecules of the carbon nanotube-proto-product.

### Claim 19 (depends on 18)

The method of claim 18, wherein forming the aligned carbon nanotube product includes, after exposing the carbon nanotube-proto-product to the infrared radiation source, an intermediate alignment step imposing further alignment on carbon nanotube molecules of the carbon nanotube-proto-product in a partially solidified state.

### Claim 20 (depends on 1)

The method of claim 1, wherein exposing the carbon nanotube proto-product to a chemical coagulant includes exposing the carbon nanotube proto-product to a continuously renewed fluid film comprising the chemical coagulant.

### Claim 21 (depends on 1)

The method of claim 1, wherein forming the aligned carbon nanotube product includes, after exposing the carbon nanotube-proto-product to the infrared radiation source and the chemical coagulant, a solid state alignment step imposing further alignment on carbon nanotube molecules of the carbon nanotube-proto-product.