# US 11,299,397 B2 · 3D self-assembled multi-modal carbon-based particles integrated into a continuous electrode film layer

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- Number: US 11,299,397 B2
- Document ID: US11299397B2
- Status: Granted
- Kind: B2
- Application number: 16/785,076
- Filed: 2020-02-07
- Published: 2021-02-04
- Granted: 2022-04-12
- Earliest claimed: 2019-07-30
- Assignees: Lyten, Inc.
- Applicants: Lyten, Inc.
- Inventors: Bruce Lanning; Michael W. Stowell; Jerzy Gazda; Jeffrey Bell
- Web page: https://patentgrep.com/patent/US11299397B2

## CPC

- C01B 32/184: Preparation
- B01J 19/12: employing electromagnetic waves
- C01B 32/194: After-treatment
- H01M 4/13: Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M 4/133: Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 4/1393: of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 4/366: {as layered products}
- H01M 4/583: Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M 4/621: {Binders}
- H01M 4/622: {being polymers}
- H01M 4/625: {Carbon or graphite}
- H01M 10/0525: Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
- H01M 10/0562: Solid materials
- B01J 2219/0886: Gas-solid
- B01J 2219/0894: Processes carried out in the presence of a plasma
- B82Y 30/00: Nanotechnology for materials or surface science, e.g. nanocomposites
- C01B 2204/02: Single layer graphene
- C01B 2204/04: Specific amount of layers or specific thickness
- C01B 2204/22: Electronic properties
- C01B 2204/32: Size or surface area
- C01P 2004/24: Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
- C01P 2004/30: extending in three dimensions
- C01P 2004/45: Aggregated particles or particles with an intergrown morphology
- C01P 2004/53: bimodal size distribution
- C01P 2004/64: Nanometer sized, i.e. from 1-100 nanometer
- C01P 2006/16: Pore diameter
- C01P 2006/40: Electric properties
- H01M 50/46: Separators, membranes or diaphragms characterised by their combination with electrodes
- Y02E 60/10: Energy storage using batteries
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

Presently disclosed is a multi-layered carbon-based scaffolded structure having a conductive substrate. A first film is deposited on the conductive substrate and includes: a first concentration of three-dimensional (3D) carbon-based particles comprising: a plurality of conductive 3D aggregates formed of graphene sheets that are sintered together to define a 3D hierarchical open porous structure with mesoscale structuring in combination with micron-scale fractal structuring that is also configured to provide conduction between contact points of the graphene sheets. A porous arrangement is formed in the 3D hierarchical open porous structure and contains a liquid electrolyte configured to provide ion transport through a plurality of interconnected porous channels. The first film is configured to provide a first conductivity. A second film is deposited on the first film and comprising a second concentration of 3D carbon-based particles. The second film configured to provide a second conductivity lower than the first conductivity.

## Claims

### Claim 1

An electrochemical cell comprising:
an anode containing an anode active material,
a cathode containing a cathode active material,
a porous separator disposed between the anode and the cathode, and
a liquid electrolyte in contact with the anode active material and the cathode active material, at least one of the anode or the cathode comprising:
an electrically conductive substrate;
a first contiguous film deposited on the electrically conductive substrate, the first contiguous film consisting of a first concentration of three-dimensional (3D) self-assembled binder-less multi-modal mesoporous carbon-based particles in contact with each other that collectively define a first electrical conductivity for the first contiguous film, each 3D self-assembled binder-less multi-modal mesoporous carbon-based particle comprising:
a plurality of electrically conductive 3D aggregates formed of graphene sheets randomly sintered together to form a 3D hierarchical open porous structure including mesoscale structuring in combination with micron-scale fractal structuring, the plurality of electrically conductive 3D aggregates configured to provide electrical conduction between contact points of the graphene sheets; and
a porous arrangement defining a plurality of interconnected porous channels formed in the 3D hierarchical open porous structure, the porous arrangement containing the liquid electrolyte and configured to facilitate ion transport through at least some interconnected porous channels; and
a second contiguous film deposited on the first contiguous film, the second contiguous film consisting of a second concentration of 3D self-assembled binder-less multi-modal mesoporous carbon-based particles in contact with each other that collectively define a second electrical conductivity for the second contiguous film, wherein the second electrical conductivity of the second contiguous film is lower than the first electrical conductivity of the first contiguous film.

### Claim 2 (depends on 1)

The electrochemical cell of claim 1, wherein the anode active material or the cathode active material resides in pores of the anode and the cathode.

### Claim 3 (depends on 1)

The electrochemical cell of claim 1, wherein the anode active material or the cathode active material has a specific surface area between approximately 80 m2/g and approximately 2,675 m2/g.

### Claim 4 (depends on 1)

The electrochemical cell of claim 1, wherein the anode active material or the cathode active material further comprises any one or more of pre-lithiated graphene sheets, pristine graphene, graphene oxide, reduced graphene oxide, graphene fluoride, graphene chloride, graphene bromide, graphene iodide, hydrogenated graphene, nitrogenated graphene, boron-doped graphene, nitrogen doped graphene, chemically functionalized graphene, physically or chemically activated or etched versions thereof, or conductive polymer coated or grafted versions thereof.

### Claim 5 (depends on 1)

The electrochemical cell of claim 1, wherein at least some of the electrically conductive 3D aggregates are sintered together and form an open porous scaffold independent of a binder.

### Claim 6 (depends on 1)

The electrochemical cell of claim 1, wherein the 3D hierarchical open porous structure comprises an active Li intercalating structure with a specific capacity of between approximately 744 and approximately 1,116 milliampere hours per gram (mAh/g).

### Claim 7 (depends on 4)

The electrochemical cell of claim 4, wherein the chemically functionalized graphene includes a functional group imparted to the 3D hierarchical open porous structure, wherein the functional group is quinone, hydroquinone, quaternized aromatic amines, mercaptan, disulfide, sulfonate (—SO3), transition metal oxide, transition metal sulfide, or any combination thereof.

### Claim 8 (depends on 1)

The electrochemical cell of claim 1, wherein the electrically conductive substrate is a current collector.

### Claim 9 (depends on 8)

The electrochemical cell of claim 8, wherein the current collector includes metal foam, metal web, metal screen, perforated metal, sheet-based 3D structure, metal fiber mat, metal nanowire mat, conductive polymer nanofiber mat, conductive polymer foam, conductive polymer-coated fiber foam, carbon foam, graphite foam, carbon aerogel, carbon xerogel, graphene foam, graphene oxide foam, reduced graphene oxide foam, carbon fiber foam, graphite fiber foam, exfoliated graphite foam, or any combination thereof.

### Claim 10 (depends on 1)

The electrochemical cell of claim 1, wherein the anode active material or the cathode active material further comprises one or more of a plurality of nanoparticles, a plurality of nanodiscs, a plurality of nanoplatelets, a plurality of nano-coatings, or a plurality of nanosheets of an inorganic material.

### Claim 11 (depends on 10)

The electrochemical cell of claim 10, wherein the plurality of nanoparticles, the plurality of nanodiscs, the plurality of nanoplatelets, the plurality of nano-coatings, or the plurality of nanosheets of an inorganic material include bismuth selenide or bismuth telluride, transition metal dichalcogenide or trichalcogenide, sulfide, selenide, telluride of a transition metal, boron nitride, or any combination thereof.

### Claim 12 (depends on 11)

The electrochemical cell of claim 11, wherein the nanoplatelets each have a thickness less than between 5 nanometers (nm) and 10 nm and a width between 1 micrometer (μm) and 5 μm.

### Claim 13 (depends on 1)

The electrochemical cell of claim 1, wherein the first electrical conductivity is between approximately 500 Siemens per meter (S/m) and approximately 20,000 S/m.

### Claim 14 (depends on 1)

The electrochemical cell of claim 1, wherein the second electrical conductivity is between 100 Siemens per meter (S/m) and 500 S/m.

### Claim 15 (depends on 1)

The electrochemical cell of claim 1, wherein the first contiguous film has an average thickness between approximately 10 micrometers (μm) and approximately 200 μm.

### Claim 16 (depends on 1)

The electrochemical cell of claim 1, wherein the second contiguous film has an average thickness between approximately 10 micrometers (μm) and approximately 200 μm.