# US 12,006,217 B2 · Method for producing microporous carbon material

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- Number: US 12,006,217 B2
- Document ID: US12006217B2
- Status: Granted
- Kind: B2
- Application number: 18/552,040
- Filed: 2022-03-16
- Published: 2024-03-21
- Granted: 2024-06-11
- Earliest claimed: 2021-03-24
- Assignees: Skeleton Technologies AG
- Applicants: Skeleton Technologies GmbH
- Inventors: Markarian Ohannes Yeghia Ohannes; Markus Klose; Daniel Weingarth; Jaan Leis
- Web page: https://patentgrep.com/patent/US12006217B2

## CPC

- C01B 32/05: Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
- B01J 8/1809: {Controlling processes}
- B01J 8/24: according to "fluidised-bed" technique (B01J8/20 takes precedence)
- C01B 32/914: Carbides of single elements
- C01B 32/921: Titanium carbide
- C01B 32/956: Silicon carbide
- B01J 2208/00017: Controlling the temperature
- B01J 2208/00539: Pressure
- C01P 2004/03: obtained by SEM
- C01P 2004/51: Particles with a specific particle size distribution
- 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
- C01P: INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS

## Abstract

Processes for the production of microporous carbon material, for use in electrodes of supercapacitors and secondary batteries, in which particulate metal carbide material is fluidized with a halogen gas at a high temperature in a fluidized bed reactor, the halogen gas is desorbed at a lower temperature of 150° C. to at most 250° C. under vacuum, and then the material is passivated using hydrogen gas and then milled.

## Claims

### Claim 1

A method for manufacturing microporous carbon material, the method comprising the steps of:
a) in a fluidized bed reactor, fluidizing a granular metal carbide material with a halogen gas or a gas mixture containing a halogen gas at a temperature of including 800° C. up to and including 1300° C.;
b) maintaining a product obtained from step a) at a temperature of including 150° C. to at most 250° C. and under vacuum at a pressure of including 1 mbar to including 300 mbar; and thereafter or subsequently
c) maintaining the product under an atmosphere of a hydrogen gas or a gas mixture containing at least 30% by volume of hydrogen based on a total volume of the gas mixture at a temperature of including 800° C. up to and including 1300° C.; and
d) comminuting the product to a D90 particle size of including 10 μm to including 30 μm and a D10 particle size of including 1.5 μm to 2 μm.

### Claim 2 (depends on 1)

The method of claim 1, wherein step a) comprises, after fluidizing with the halogen gas or gas mixture, fluidizing with a purge gas in the fluidized bed reactor at a temperature of including 800° C. to including 1300° C., wherein the purge gas does not react with at least carbon at said temperature.

### Claim 3 (depends on 2)

The method of claim 2, wherein the purge gas is selected from a group consisting of: helium, neon, argon, krypton, and xenon.

### Claim 4 (depends on 2)

The method of claim 2, wherein the purge gas is argon.

### Claim 5 (depends on 1)

The method of claim 1, wherein the granular metal carbide material is selected from a group consisting of: vanadium carbide material, titanium carbide material, molybdenum carbide material, silicon carbide material, tungsten carbide material, tantalum carbide material, and niobium carbide material.

### Claim 6 (depends on 1)

The method of claim 1, wherein the granular metal carbide material is silicon carbide material and wherein the halogen gas is chlorine.

### Claim 7 (depends on 1)

The method of claim 1, wherein in step a) the halogen gas is supplied in an amount which is from both including 100% to including 110% of the stoichiometrically required amount.

### Claim 8 (depends on 1)

The method according to claim 1, wherein in step b) the pressure is from including 5 mbar to including 200 mbar, or from including 5 mbar to including 80 mbar, or preferably from including 8 mbar to 15 mbar.

### Claim 9 (depends on 1)

The method according to claim 1, wherein:
step a) is carried out for a duration of from including 8 hours to including 13 hours;
step b) is performed for a duration of from including 12 hours to including 30 hours; and
step c) is performed for a duration of from including 2 hours to including 4 hours.

### Claim 10 (depends on 9)

The method of claim 9, wherein:
in step a) fluidizing with halogen gas is performed for a duration of including 9 hours up to and including 11 hours, and fluidizing with a purge gas is performed for a duration of 1.5 hours up to 2.5 hours; and
step b) is carried out for a duration of from including 22 hours to including 26 hours.

### Claim 11 (depends on 1)

The method according to claim 1, wherein step c) is carried out before step d), or wherein step d) is carried out before step c), or wherein step c) is carried out before step d) and then step c) is carried out again for a shorter duration.

### Claim 12 (depends on 1)

The method according to claim 1, wherein step b) is carried out using the fluidized bed reactor.

### Claim 13 (depends on 1)

The method according to claim 1, wherein step c) is carried out using the fluidized bed reactor or using a rotary kiln.