Laser-induced graphene (LIG) and laser induced graphene scrolls (LIGS) materials

Patent metadata

Field	Value
Publication number	US-11014816-B2
Application number	US-201716312837-A
Country	US
Kind code	B2
Filing date	Jun 21, 2017
Priority date	Jun 21, 2016
Publication date	May 25, 2021
Grant date	May 25, 2021

Abstract

Laser-induced graphene (LIG) and laser-induced graphene scrolls (LIGS) materials and, more particularly to LIGS, methods of making LIGS (such as from polyimide (PI)), laser-induced removal of LIG and LIGS, and 3D printing of LIG and LIGS using a laminated object manufacturing (LOM) process.

First claim

What is claimed is:

1. A method comprising exposing a graphene precursor material to a laser source to form laser-induced graphene scrolls (LIGS) material, wherein
(a) the LIGS material comprises scrolls of graphene;
(b) the LIGS material is derived from the graphene precursor material; and
(c) the graphene precursor material comprises a polymer.

2. The method of claim 1 , wherein the polymer is selected from a group consisting of polymer films, polymer fibers, polymer monoliths, polymer powders, polymer blocks, optically transparent polymers, homopolymers, vinyl polymers, chain-growth polymers, step-growth polymers, condensation polymers, random polymers, ladder polymers, semi-ladder polymers, block co-polymers, carbonized polymers, aromatic polymers, cyclic polymers, doped polymers, polyimide (PI), polyetherimide (PEI), polyether ether ketone (PEEK), polyamide (PA), polybenzoxazole (PBO), polyaramids, and polymer composites and combinations thereof.

3. The method of claim 1 , wherein the polymer comprises polyimide.

4. The method of claim 1 , wherein
(a) the step of exposing comprises tuning one or more parameters of the laser source; and
(b) the tuning of the one or more parameters of the laser source comprises modifying the laser wavelength so that the laser wavelength is at an absorption band of the graphene precursor material.

5. The method of claim 1 , wherein
(a) the step of exposing comprises tuning one or more parameters of the laser source; and
(b) the one or more parameters of the laser source are selected from a group consisting of laser wavelength, laser power, laser energy density, laser pulse width, gas environment, gas pressure, gas flow rate, direction of gas flow relative to the lasing head, and combinations thereof.

6. The method of claim 1 , wherein the laser source has a wavelength ranging from about 20 nm to about 100 μm.

7. The method of claim 1 , wherein the laser source comprises near-field scanning optical microscopy.

8. The method of claim 1 , wherein the laser source comprises a laser having a beam that is diffused with a lens or series of lenses.

9. The method of claim 8 , wherein the laser has a high powered beam that can cover an exposed area that is a large area or line such that the diffused energy has a fluence capable to form the LIGS over the entire exposed area.

10. The method of claim 1 , wherein the laser source has a power ranging from about 1 W to about 100 W.

11. The method of claim 1 , wherein the polymer comprises a doped polymer.

12. The method of claim 11 , wherein the doped polymer comprises a dopant selected from a group consisting of heteroatoms, metals, metal oxides, metal chalcogenides, metal nanoparticles, metal salts, organic additives, inorganic additives, metal organic compounds, and combinations thereof.

13. The method of claim 1 , wherein the LIGS material comprises a doped LIGS material.

14. The method of claim 13 , wherein the doped graphene comprises a dopant selected from a group consisting of heteroatoms, metals, metal oxides, metal nanoparticles, metal chalcogenides, metal salts, organic additives, inorganic additives, and combinations thereof.

15. The method of claim 1 , wherein
(a) the laser source has a laser fluence of at least about 20 J/cm 2 , and
(b) the laser source has a wavelength of at least about 9.3 μm.

16. The method of claim 1 , wherein the laser source has a laser fluence of more than about 40 J/cm 2 .

17. The method of claim 1 , wherein the LIGS material has a thickness of at least about 20 μm.

18. The method of claim 1 , wherein the LIGS material are formed in a one-step laser thermolysis process at a radiation level of at least about 20 J/cm 2 .

19. The method of claim 1 , wherein
(a) the laser source is operable above a critical fluence point needed to initiate carbonization of the graphene precursor material; and
(b) the critical fluence point of the laser is at least about 5 J/cm 2 .

20. The method of claim 1 , wherein the laser source is a laser that is being operated in raster mode.

21. The method of claim 1 , wherein the laser source is a laser that is being operated in vector mode.

22. The method of claim 1 , wherein the laser source has a pulse density such that the pulses do not overlap.

23. A method comprising exposing a graphene precursor material to a laser source to form laser-induced graphene scrolls (LIGS) material, wherein
(a) the LIGS material comprises scrolls of graphene;
(b) the LIGS material is derived from the graphene precursor material; and
(c) the LIGS material comprises nanoscrolls of graphene having an average diameter in a range from about 10 nm to about 500 nm.

24. A method comprising:
(i) exposing a graphene precursor material to a laser source to form laser-induced graphene scrolls (LIGS) material, wherein
(a) the LIGS material comprises scrolls of graphene, and
(b) the LIGS material is derived from the graphene precursor material; and

(ii) incorporating the LIGS material into an electronic device.

25. The method of claim 24 , wherein the electronic device comprises an electrode comprising the LIGS material.

26. The method of claim 24 , wherein the electronic device is a flexible electronic device.

27. The method of claim 24 , wherein the electronic device is an energy storage device or an energy generation device.

28. The method of claim 24 , wherein the electronic device is selected from a group consisting of supercapacitors, micro-supercapacitors, pseudo capacitors, batteries, micro batteries, lithium-ion batteries, sodium-ion batteries, magnesium-ion batteries, electrodes, conductive electrodes, sensors, lithium ion capacitors, photovoltaic devices, electronic circuits, fuel cell devices, thermal management devices, biomedical devices, and combinations thereof.

29. The method of claim 24 further comprising a step of associating the electronic device with an electrolyte.

Assignees

• Univ Rice William M

Inventors

• Tour James M
• Luong Duy X
• Subramanian Ajay

Classifications

• H10P14/20

  of semiconductor materials · CPC title

• H10P14/3406

  Carbon, e.g. diamond-like carbon · CPC title

• H10D62/882

  Graphene · CPC title

• B01D71/0211

  Graphene or derivates thereof · CPC title

• B01D71/0212

  Carbon nanotubes · CPC title