# US 11,306,401 B2 · Methods and apparatuses for production of carbon, carbide electrodes, and carbon compositions

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- Number: US 11,306,401 B2
- Document ID: US11306401B2
- Status: Granted
- Kind: B2
- Application number: 15/866,660
- Filed: 2018-01-10
- Published: 2018-07-12
- Granted: 2022-04-19
- Earliest claimed: 2014-10-21
- Assignees: West Virginia University Research Corporation
- Applicants: West Virginia University Research Corporation
- Inventors: Alfred H. Stiller; Christopher L. Yurchick
- Web page: https://patentgrep.com/patent/US11306401B2

## CPC

- C25B 1/00: Electrolytic production of inorganic compounds or non-metals
- C01B 32/00: Carbon; Compounds thereof (C01B21/00, C01B23/00 take precedence; percarbonates C01B15/10; carbon black C09C1/48)
- C01B 32/05: Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
- C01B 32/182: Graphene
- C01B 32/184: Preparation
- C01B 32/20: Graphite
- C01B 32/25: Diamond
- C25B 1/135: Carbon
- C25B 11/043: Carbon, e.g. diamond or graphene
- H01B 1/04: mainly consisting of carbon-silicon compounds, carbon or silicon
- H04W 28/26: Resource reservation
- H04W 72/0453: Resources in frequency domain, e.g. a carrier in FDMA
- H04W 72/1215: {for collaboration of different radio technologies}
- H04W 72/20: Control channels or signalling for resource management
- H04W 74/002: {Transmission of channel access control information}
- B82Y 40/00: Manufacture or treatment of nanostructures
- C01B 2204/22: Electronic properties
- H04W 16/14: Spectrum sharing arrangements {between different networks}
- H04W 48/16: Discovering, processing access restriction or access information
- H04W 88/06: adapted for operation in multiple networks {or having at least two operational modes}, e.g. multi-mode terminals
- H04W 88/10: adapted for operation in multiple networks, e.g. multi-mode access points
- C25B: ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR (anodic or cathodic protection C23F13/00; single-crystal growth C30B)
- C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C}
- H01B: CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES (selection for magnetic properties H01F1/00; waveguides H01P {; printed circuits H05K})
- H04W: WIRELESS COMMUNICATION NETWORKS (broadcast communication H04H; communication systems using wireless links for non-selective communication, e.g. wireless extensions H04M1/72)
- B82Y: SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES

## Abstract

An apparatus containing at least one electrochemical cell with an electrode structure. The electrode structure contains at least one carbide chemical compound. The carbide chemical compound may be a salt-like carbide. The electrode may contain at least one electronically conductive element different from the carbide. Carbon compositions of various forms may be formed by the methods and apparatus using the electrode structure. Large pieces of pure carbon may be produced. Post-reaction processing of the carbon may be carried out such as exfoliation.

## Claims

### Claim 1

An apparatus comprising at least one electrochemical cell comprising:
at least one anode comprising at least one carbide chemical compound, and
at least one cathode,
wherein the electrochemical cell apparatus is a galvanic cell apparatus and is capable of producing an elemental carbon material, and
wherein the carbide chemical compound is a salt-like carbide, an aluminum carbide, or a beryllium carbide.

### Claim 2 (depends on 1)

The apparatus of claim 1, wherein the carbide chemical compound has an electronic conductivity of at least 10−8 S/cm.

### Claim 3 (depends on 1)

The apparatus of claim 1, wherein the carbide chemical compound is in the form of individual pieces or particles.

### Claim 4 (depends on 1)

The apparatus of claim 1, wherein the carbide chemical compound is in the form of individual pieces or particles having a size of less than one cm.

### Claim 5 (depends on 1)

The apparatus of claim 1, wherein the carbide chemical compound contacts at least one electrically conductive material.

### Claim 6 (depends on 1)

The apparatus of claim 1, wherein the carbide chemical compound is held in an electrically conductive container.

### Claim 7 (depends on 1)

The apparatus of claim 1, wherein the electrochemical cell apparatus cathode is a metal cathode.

### Claim 8 (depends on 1)

The apparatus of claim 1, wherein the electrochemical cell apparatus comprises at least one salt bridge or at least one ion exchange membrane.

### Claim 9 (depends on 1)

The apparatus of claim 1, wherein the electrochemical cell apparatus comprises an external voltage source to regulate an oxidation reaction of carbide in the carbide chemical compound.

### Claim 10 (depends on 1)

The apparatus of claim 1, wherein the apparatus further comprises at least one solution comprising at least one solvent and at least one dissolved salt, and the solution is free of dissolved carbide chemical compound.

### Claim 11 (depends on 1)

The apparatus of claim 1, wherein the anode comprises at least one electronically conductive structural element different from the carbide chemical compound and contacting the at least one carbide chemical compound.

### Claim 12 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound is methanide, acetylide, or sesquicarbide.

### Claim 13 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound is calcium carbide, aluminum carbide, sodium carbide, magnesium carbide, lithium carbide, or beryllium carbide.

### Claim 14 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound is in the form of individual pieces or particles having a size of less than one cm.

### Claim 15 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound is in the form of individual pieces or particles having a size of at least one micron.

### Claim 16 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound is divided into separate portions which are each contacted with at least one electrically conductive structural element.

### Claim 17 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound is at least about 95% pure.

### Claim 18 (depends on 11)

The apparatus of claim 11, wherein the electronically conductive structural element is a binder for the carbide chemical compound.

### Claim 19 (depends on 11)

The apparatus of claim 11, wherein the electronically conductive structural element is a container and the carbide chemical compound is held in the container.

### Claim 20 (depends on 11)

The apparatus of claim 11, wherein the electronically conductive structural element is a container and the carbide chemical compound is held in the container, and the container has openings which allow fluid to enter the container and contact the carbide chemical compound.

### Claim 21 (depends on 11)

The apparatus of claim 11, wherein the electronically conductive structural element is a metallic container and the carbide chemical compound is held in the metallic container.

### Claim 22 (depends on 11)

The apparatus of claim 11, wherein the electronically conductive structural element comprises at least one conductive rod.

### Claim 23 (depends on 11)

The apparatus of claim 11, wherein the electronically conductive structural element of the electrode structure comprises at least one current collector.

### Claim 24 (depends on 11)

The apparatus of claim 11, wherein the electrode structure is adapted for use as an anode in an electrochemical cell apparatus for production of the elemental carbon material.

### Claim 25 (depends on 11)

The apparatus of claim 11, wherein the electrode structure is adapted for use as an anode in a galvanic cell apparatus for production of the elemental carbon material.

### Claim 26 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound has an electronic conductivity of at least 10−8 S/cm.

### Claim 27 (depends on 11)

The apparatus of claim 11, wherein the carbide chemical compound is in the form of individual pieces or particles.

### Claim 28 (depends on 1)

The apparatus of claim 1, wherein each of the at least one anode and the at least one cathode is contacted with a solution comprising at least one organic solvent and at least one dissolved salt.

### Claim 29

An apparatus comprising at least one electrochemical cell comprising:
at least one anode comprising at least one carbide chemical compound, and
at least one cathode,
wherein the electrochemical cell apparatus is a galvanic cell apparatus and is capable of producing an elemental carbon material, and
wherein the carbide chemical compound is in the form of individual pieces or particles having a size of less than one cm.

### Claim 30 (depends on 29)

The apparatus of claim 29, wherein the carbide chemical compound is a salt-like carbide or an intermediate transition metal carbide.

### Claim 31 (depends on 29)

The apparatus of claim 29, wherein the carbide chemical compound is a salt-like carbide.

### Claim 32 (depends on 29)

The apparatus of claim 29, wherein the carbide chemical compound is calcium carbide or aluminum carbide.

### Claim 33 (depends on 29)

The apparatus of claim 29, wherein the carbide chemical compound contacts at least one electrically conductive material.

### Claim 34 (depends on 29)

The apparatus of claim 29, wherein the electrochemical cell apparatus cathode is a metal cathode.

### Claim 35 (depends on 29)

The apparatus of claim 29, wherein the electrochemical cell apparatus comprises at least one salt bridge or at least one ion exchange membrane.

### Claim 36 (depends on 29)

The apparatus of claim 29, wherein the electrochemical cell apparatus comprises an external voltage source to regulate an oxidation reaction of carbide in the carbide chemical compound.

### Claim 37 (depends on 29)

The apparatus of claim 29, wherein the apparatus further comprises at least one solution comprising at least one solvent and at least one dissolved salt, and the solution is free of dissolved carbide chemical compound.

### Claim 38 (depends on 29)

The apparatus of claim 29, wherein the anode comprises at least one electronically conductive structural element different from the carbide chemical compound and contacting the at least one carbide chemical compound.

### Claim 39 (depends on 29)

The apparatus of claim 29, wherein each of the at least one anode and the at least one cathode is contacted with a solution comprising at least one organic solvent and at least one dissolved salt.