# US 10,373,808 B2 · Seedless particles with carbon allotropes

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- Number: US 10,373,808 B2
- Document ID: US10373808B2
- Status: Granted
- Kind: B2
- Application number: 16/003,680
- Filed: 2018-06-08
- Published: 2018-10-11
- Granted: 2019-08-06
- Earliest claimed: 2017-02-09
- Assignees: Lyten, Inc.
- Applicants: Lyten, Inc.
- Inventors: Bryce H. Anzelmo; Daniel Cook; Hossein-Ali Ghezelbash; Shreeyukta Singh; Michael W. Stowell; David Tanner
- Web page: https://patentgrep.com/patent/US10373808B2

## CPC

- H01J 37/32192: {Microwave generated discharge (H01J37/32357, H01J37/32366, H01J37/32394, H01J37/32403 take precedence)}
- C01B 32/00: Carbon; Compounds thereof (C01B21/00, C01B23/00 take precedence; percarbonates C01B15/10; carbon black C09C1/48)
- C01B 32/15: Nano-sized carbon materials
- C01B 32/152: Fullerenes
- C01B 32/182: Graphene
- C01B 32/19: by exfoliation
- H01J 37/3244: {Gas supply means}
- H01J 37/32532: {Electrodes}
- C01P 2004/50: Agglomerated particles
- C01P 2004/51: Particles with a specific particle size distribution
- C01P 2006/12: Surface area
- C01P 2006/40: Electric properties
- H01J 2237/334: Etching
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Carbon materials having carbon aggregates, where the aggregates include carbon nanoparticles and no seed particles, are disclosed. In various embodiments, the nanoparticles include graphene, optionally with multi-walled spherical fullerenes and/or another carbon allotrope. In various embodiments, the nanoparticles and aggregates have different combinations of: a Raman spectrum with a 2D-mode peak and a G-mode peak, and a 2D/G intensity ratio greater than 0.5, a low concentration of elemental impurities, a high Brunauer-Emmett and Teller (BET) surface area, a large particle size, and/or a high electrical conductivity. Methods are provided to produce the carbon materials.

## Claims

### Claim 1

A carbon material comprising:
a plurality of carbon aggregates, each carbon aggregate comprising a plurality of carbon nanoparticles, each carbon nanoparticle comprising graphene, with no seed particles;
wherein:
the graphene in the plurality of carbon nanoparticles comprises up to 15 layers;
a median size of the carbon aggregates that comprise the carbon nanoparticles is from 1 micron to 50 microns;
a surface area of the carbon aggregates is from 50 m2/g to 300 m2/g, when measured via a Brunauer-Emmett-Teller (BET) method with nitrogen as the adsorbate; and
the carbon aggregates, when compressed, have an electrical conductivity from 500 S/m to 20,000 S/m.

### Claim 2 (depends on 1)

The carbon material of claim 1, further comprising one or more other carbon allotropes in addition to graphene, wherein a percentage of the graphene to the other carbon allotropes is greater than 90%.

### Claim 3 (depends on 1)

The carbon material of claim 1, wherein a Raman spectrum of the carbon material, using 532 nm incident light, comprises: a 2D-mode peak; a G-mode peak; and a 2D/G intensity ratio greater than 0.5.

### Claim 4 (depends on 1)

The carbon material of claim 1, further comprising amorphous carbon, wherein:
a percentage of the amorphous carbon to the graphene is less than 5%; and
a Raman spectrum of the carbon material comprising the amorphous carbon, using 532 nm incident light, comprises: a 2D-mode peak; a D-mode peak; a G-mode peak; a D/G intensity ratio greater than 0.5; a low intensity 2D-mode peak; and a shallow valley between the D-mode peak and G-mode peak.

### Claim 5 (depends on 1)

The carbon material of claim 1, wherein the carbon aggregates are post-processed using a method selected from the group consisting of milling, grinding, exfoliating, annealing, sintering, steaming, filtering, lypolizing, doping, and adding elements.

### Claim 6 (depends on 5)

The carbon material of claim 5, wherein the surface area of the post-processed carbon aggregates is from 50 m2/g to 1000 m2/g, when measured using the BET method with nitrogen as the adsorbate.

### Claim 7 (depends on 1)

The carbon material of claim 1, wherein the graphene has a 3D structure.

### Claim 8 (depends on 1)

An electrically conductive ink comprising the carbon material of claim 1 and liquids.

### Claim 9 (depends on 1)

A tire additive comprising the carbon material of claim 1.

### Claim 10 (depends on 1)

A battery electrode comprising the carbon material of claim 1.

### Claim 11

A carbon material comprising:
a plurality of carbon aggregates, each carbon aggregate comprising a plurality of carbon nanoparticles, each carbon nanoparticle comprising graphene and multi-walled spherical fullerenes, with no seed particles;
wherein:
the graphene in the plurality of carbon nanoparticles comprises up to 15 layers;
a Raman spectrum of the carbon material comprising the multi-walled spherical fullerenes, using 532 nm incident light, comprises: a D-mode peak; a G-mode peak; and a D/G intensity ratio less than 1.2;
a median size of the carbon aggregates that comprise the carbon nanoparticles is from 1 micron to 100 microns;
a surface area of the carbon aggregates is at least from 10 m2/g to 300 m2/g, when measured using a Brunauer-Emmett-Teller (BET) method with nitrogen as the adsorbate; and
the carbon aggregates, when compressed, have an electrical conductivity at least from 500 S/m to 20,000 S/m.

### Claim 12 (depends on 11)

The carbon material of claim 11, wherein the D/G intensity ratio is from 0.9 to 1.1.

### Claim 13 (depends on 11)

The carbon material of claim 11, wherein a percentage of the multi-walled spherical fullerenes to the graphene is from 20% to 80%.

### Claim 14 (depends on 11)

The carbon material of claim 11, wherein the multi-walled spherical fullerenes comprise connected multi-walled spherical fullerenes, in which at least some of the multi-walled spherical fullerenes are coated by layers of the graphene.

### Claim 15 (depends on 11)

The carbon material of claim 11, wherein the carbon aggregates are post-processed using a method selected from the group consisting of milling, grinding, exfoliating, annealing, sintering, steaming, filtering, lypolizing, doping, and adding elements.

### Claim 16 (depends on 15)

The carbon material of claim 15, wherein the surface area of the post-processed carbon aggregates is from 50 m2/g to 500 m2/g, when measured using the BET method with nitrogen as the adsorbate.

### Claim 17 (depends on 11)

The carbon material of claim 11, wherein the graphene has a 3D structure.

### Claim 18

A carbon material comprising:
a plurality of carbon aggregates, each carbon aggregate comprising a plurality of carbon nanoparticles, each carbon nanoparticle comprising a mixture of graphene and at least one other carbon allotrope, with no seed particles;
wherein:
the graphene in the plurality of carbon nanoparticles comprises up to 15 layers;
a median size of the carbon aggregates that comprise the carbon nanoparticles is from 1 micron to 100 microns;
a surface area of the carbon aggregates is from 10 m2/g to 300 m2/g, when measured using a Brunauer-Emmett-Teller (BET) method with nitrogen as the adsorbate; and
the carbon aggregates, when compressed, have an electrical conductivity at least from 100 S/m to 20,000 S/m.

### Claim 19 (depends on 18)

The carbon material of claim 18, wherein a percentage of the graphene to the at least one other carbon allotrope is from 5% to 95%.

### Claim 20 (depends on 18)

The carbon material of claim 18, wherein a Raman spectrum of the carbon material comprising the graphene, using 532 nm incident light, comprises: a 2D-mode peak; a G-mode peak; and a 2D/G intensity ratio greater than 0.5.

### Claim 21 (depends on 18)

The carbon material of claim 18, wherein the at least one other carbon allotrope comprises multi-walled spherical fullerenes.

### Claim 22 (depends on 21)

The carbon material of claim 21, wherein a percentage of the graphene to the multi-walled spherical fullerenes is from 20% to 80%.

### Claim 23 (depends on 21)

The carbon material of claim 21, wherein the multi-walled spherical fullerenes comprise connected multi-walled spherical fullerenes, in which at least some of the multi-walled spherical fullerenes are coated by layers of the graphene.

### Claim 24 (depends on 18)

The carbon material of claim 18, wherein the at least one other carbon allotrope comprises amorphous carbon.

### Claim 25 (depends on 24)

The carbon material of claim 24, wherein a percentage of the graphene to the amorphous carbon is greater than 95%.

### Claim 26 (depends on 18)

The carbon material of claim 18, wherein the at least one other carbon allotrope comprises predominantly sp3 hybridization.

### Claim 27 (depends on 26)

The carbon material of claim 26, wherein the percentage of graphene to the at least one other carbon allotrope is from 5% to 95%.

### Claim 28 (depends on 18)

The carbon material of claim 18, wherein the carbon aggregates are post-processed using a method selected from the group consisting of milling, grinding, exfoliating, annealing, sintering, steaming, filtering, lypolizing, doping, and adding elements.

### Claim 29 (depends on 28)

The carbon material of claim 28, wherein the surface area of the post-processed carbon aggregates is from 50 m2/g to 2000 m2/g, when measured using the BET method with nitrogen as the adsorbate.

### Claim 30 (depends on 18)

The carbon material of claim 18, wherein the graphene has a 3D structure.