# US 12,006,223 B2 · Activated carbon electrode material > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 12,006,223 B2 - Document ID: US12006223B2 - Status: Granted - Kind: B2 - Application number: 17/293,224 - Filed: 2019-11-12 - Published: 2022-09-29 - Granted: 2024-06-11 - Earliest claimed: 2018-11-13 - Assignees: Pittsburg State University; Missouri Soybean Merchandising Council - Applicants: Pittsburg State University; Missouri Soybean Merchandising Council - Inventors: Ram Gupta; Pawan Kahol - Web page: https://patentgrep.com/patent/US12006223B2 ## CPC - C01B 32/318: characterised by the starting materials - H01M 4/587: for inserting or intercalating light metals - B01F 27/00: Mixers with rotary stirring devices in fixed receptacles (magnetic mixers B01F33/45); Kneaders - C01B 32/30: Active carbon - C01B 32/348: Metallic compounds - C01P 2002/82: by IR- or Raman-data - C01P 2002/85: by XPS, EDX or EDAX data - C01P 2006/12: Surface area - C01P 2006/16: Pore diameter - C01P 2006/40: Electric properties - Y02E 60/13: Energy storage using capacitors - C01B: NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; {METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C} - H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY - B01F: MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING (mixing paints B44D3/06) - 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 An activated carbon powder comprising activated carbon particles that comprise D-band carbon corresponding to a sp3 hybridized disordered carbon phase and G-band carbon corresponding to a sp2 hybridized graphitic phase at a controlled proportion. Additionally, the activated carbon particles comprise nitrogen at an amount that is in a range of about 0.3 atomic % to about 1.8 atomic % of the activated carbon particles, wherein at least some of the nitrogen atoms are substituted for carbon atoms in the crystal lattice structure of the G-band carbon. Also, the carbon particles have a surface area that is in a range of about 900 m2/g to about 2,500 m2/g, an average pore width in a range of about 1 nm to about 4 nm, a microporous surface area in a range of about 300 m2/g to about 1,350 m2/g, and a cumulative surface area of pores with a hydraulic radius in a range of 0.285 nm to 1.30 nm that is in a range of about 1,000 m2/g to about 3,000 m2/g. ## Claims ### Claim 1 An activated carbon powder comprising activated carbon particles, wherein the activated carbon particles have a Brunauer-Emmett-Teller (BET) surface area that is in a range of about 900 m2/g to about 2,500 m2/g, and wherein the activated carbon particles comprise: (a) carbon that comprises: (i) D-band carbon corresponding to a sp3 hybridized disordered carbon phase; and (ii) G-band carbon corresponding to a sp2 hybridized graphitic phase; wherein the D-band carbon and G-band carbon are at a proportion, determined using Raman spectroscopy to arrive at relative intensities of D-band carbon (ID) and G-band carbon (IG), such that a IG/ID ratio is in a range of 0 to about 2; (b) nitrogen at an amount, determined by X-ray photoelectron spectroscopy, that is in a range of about 0.3 atomic % to about 1.8 atomic % of the activated carbon particles, wherein at least some of the nitrogen atoms are substituted for carbon atoms in the crystal lattice structure of the G-band carbon sp2 hybridized graphitic phase; and (c) mesopores with diameters in a range of 2 nm to 5 nm and micropores with diameters less than 2 nm, the activated carbon particles having: (i) an average pore width, determined by the Barrett, Joyner, and Halenda (BJH) method, in a range of about 1 nm to about 4 nm; (ii) a microporous surface area, determined by the t-plot method, in a range of about 300 m2/g to about 1,350 m2/g; and (ii) a cumulative surface area of micropores with a hydraulic radius in a range of 0.285 nm to 1.30 nm that is in a range of about 1,000 m2/g to about 3,000 m2/g. ### Claim 2 (depends on 1) The activated carbon powder of claim 1, wherein: the BET surface area of the activated carbon particles is in a range of about 1,300 m2/g to about 2,200 m2/g; the IG/ID ratio is in a range of about 0 to about 1.5; the amount of nitrogen is in a range of about 0.5 atomic % to about 1.7 atomic % of the activated carbon particles; the microporous surface area, determined by the t-plot method, is in a range of about 600 m2/g to about 1,200 m2/g; and the cumulative surface area of micropores with a hydraulic radius in a range of 0.285 nm to 1.30 nm is in a range of about 1,400 m2/g to about 2,600 m2/g. ### Claim 3 (depends on 1) The activated carbon powder of claim 1, wherein the average pore width, determined by the BJH method, is in a range of about 2 nm to about 4 nm. ### Claim 4 (depends on 1) The activated carbon powder of claim 1, wherein the average pore width, determined by the BJH method, is in a range of about 1 nm to about 2 nm. ### Claim 5 (depends on 1) The activated carbon powder of claim 1, wherein the activated carbon particles have a specific capacitance (Csp), at a current density of 1 A/g, that is in a range of about 130 F/g to about 330 F/g. ### Claim 6 (depends on 1) The activated carbon powder of claim 1, wherein the activated carbon particles have a specific capacitance, at a current density of 1 A/g, that is in a range of about 100 F/g to about 250 F/g. ### Claim 7 A process for producing activated carbon particles of an activated carbon powder, the process comprising: conducting an activation-pyrolyzation treatment of a precursor that comprises a uncarbonized plant material powder, a partially carbonized plant material powder, or a combination thereof, wherein the activation-pyrolyzation treatment comprises: mixing the precursor with an activating agent to form a precursor-activating agent mixture, wherein the activating agent is selected to react with carbon in the precursor during the activation-pyrolyzation treatment thereby forming one or more products that are suitable to be removed during a washing treatment conducted after the activation-pyrolyzation treatment; and combinations thereof; and heating the precursor-activating agent mixture in a pyrolyzation inert atmosphere at a pyrolyzation temperature and for a pyrolyzation duration sufficient to complete the carbonization of the precursor thereby forming an activated-pyrolyzed material; and conducting a washing treatment of the activated-pyrolyzed material with one or more washing liquids suitable to reduce or remove the one or more products of the reaction between carbon and the activating agent from the activated-pyrolyzed material thereby forming the activated carbon particles of the activated carbon powder, wherein the activated carbon particles have a Brunauer-Emmett-Teller (BET) surface area that is in a range of about 900 m2/g to about 2,500 m2/g, and wherein the activated carbon particles comprise: (a) carbon that comprises: (i) D-band carbon corresponding to a sp3 hybridized disordered carbon phase; and (ii) G-band carbon corresponding to a sp2 hybridized graphitic phase; wherein the D-band carbon and G-band carbon are at a proportion, determined using Raman spectroscopy to arrive at relative intensities of D-band carbon (ID) and G-band carbon (IG), such that a IG/ID ratio is in a range of 0 to about 2; (b) nitrogen at an amount, determined by X-ray photoelectron spectroscopy, that is in a range of about 0.3 atomic % to about 1.8 atomic % of the activated carbon particles, wherein at least some of the nitrogen atoms are substituted for carbon atoms in the crystal lattice structure of the G-band carbon sp2 hybridized graphitic phase; and (c) mesopores with diameters in a range of 2 nm to 5 nm and micropores with diameters less than 2 nm, the activated carbon particles having: (i) an average pore width, determined by the Barrett, Joyner, and Halenda (BJH) method, in a range of about 1 nm to about 4 nm; (ii) a microporous surface area, determined by the t-plot method, in a range of about 300 m2/g to about 1,350 m2/g; and (iii) a cumulative surface area of micropores with a hydraulic radius in a range of 0.285 nm to 1.30 nm that is in a range of about 1,000 m2/g to about 3,000 m2/g. ### Claim 8 (depends on 7) The process of claim 7 further comprising: conducting a thermal pretreatment before the activation-pyrolyzation treatment, wherein the thermal pretreatment comprises heating the uncarbonized plant material powder in a pretreatment inert atmosphere at a pretreatment temperature and for a pretreatment duration sufficient to release volatile, low-stability molecules within the uncarbonized plant material powder thereby producing a partially carbonized plant material powder suitable for the activation-pyrolyzation treatment. ### Claim 9 (depends on 7) The process of claim 7, wherein the precursor consists of the uncarbonized plant material powder or the partially carbonized plant material powder. ### Claim 10 (depends on 7) The process of claim 7, wherein: the activating agent is selected from the group consisting of KOH, NaOH, ZnCl2, H3PO4, steam, and combinations thereof; and the plant material powder is derived from non-grain soybean plant parts, orange peels, banana peels, tea leaves, corn stover, and combinations thereof. ### Claim 11 (depends on 7) The process of claim 7, wherein the activating agent is KOH, and the precursor and the activating agent are at a mass ratio that is in a range of about 1:0.5 to about 1:3. ### Claim 12 (depends on 7) The process of claim 7, wherein at least one of the washing liquids of the washing treatment is a solution comprising HCl solution and deionized water and wherein a subsequent washing liquid is deionized water. ### Claim 13 (depends on 7) The process of claim 7, wherein: the pretreatment inert atmosphere is selected from the group consisting of nitrogen, argon, and combinations thereof; the pretreatment temperature is in a range of about 250° C. to about 500° C.; and the pretreatment duration is in a range of about 1 hour to about 2 hours. ### Claim 14 (depends on 7) The process of claim 7, wherein: the precursor and activating agent are at a mass ratio in a range of about 1:0.5 to 1:3; the pyrolyzation atmosphere is selected from the group consisting of nitrogen, argon, and combinations thereof; the pyrolyzation temperature is in a range of about 600° C. to about 900° C.; and the pyrolyzation duration is in a range of about 1 hour to about 2 hours. ### Claim 15 (depends on 7) The process of claim 7, wherein: the precursor and activating agent are at a mass ratio in a range of about 1:0.125 to 1:1; the pyrolyzation atmosphere is selected from the group consisting of nitrogen, argon, and combinations thereof; the pyrolyzation temperature is in a range of about 700° C. to about 850° C.; and the pyrolyzation duration is in a range of about 1 hour to about 2 hours. ### Claim 16 (depends on 7) The process of claim 7, wherein the plant material powder is derived from non-grain soybean plant parts selected from the group consisting of shells, stems, leaves, and combinations thereof. ### Claim 17 An electrode comprising an activated carbon powder comprising activated carbon particles, wherein the activated carbon particles have a Brunauer-Emmett-Teller (BET) surface area that is in a range of about 900 m2/g to about 2,500 m2/g, and wherein the activated carbon particles comprise: (a) carbon that comprises: (i) D-band carbon corresponding to a sp3 hybridized disordered carbon phase; and (ii) G-band carbon corresponding to a sp2 hybridized graphitic phase; wherein the D-band carbon and G-band carbon are at a proportion, determined using Raman spectroscopy to arrive at relative intensities of D-band carbon (ID) and G-band carbon (IG), such that a IG/ID ratio is in a range of 0 to about 2; (b) nitrogen at an amount, determined by X-ray photoelectron spectroscopy, that is in a range of about 0.3 atomic % to about 1.8 atomic % of the activated carbon particles, wherein at least some of the nitrogen atoms are substituted for carbon atoms in the crystal lattice structure of the G-band carbon sp2 hybridized graphitic phase; and (c) mesopores with diameters in a range of 2 nm to 5 nm and micropores with diameters less than 2 nm, the activated carbon particles having: (i) an average pore width, determined by the Barrett, Joyner, and Halenda (BJH) method, in a range of about 1 nm to about 4 nm; (ii) a microporous surface area, determined by the t-plot method, in a range of about 300 m2/g to about 1,350 m2/g; and (ii) a cumulative surface area of micropores with a hydraulic radius in a range of 0.285 nm to 1.30 nm that is in a range of about 1,000 m2/g to about 3,000 m2/g. ### Claim 18 A battery or supercapacitor comprising an electrode comprising an activated carbon powder comprising activated carbon particles, wherein the activated carbon particles have a Brunauer-Emmett-Teller (BET) surface area that is in a range of about 900 m2/g to about 2,500 m2/g, and wherein the activated carbon particles comprise: (a) carbon that comprises: (i) D-band carbon corresponding to a sp3 hybridized disordered carbon phase; and (ii) G-band carbon corresponding to a sp2 hybridized graphitic phase; wherein the D-band carbon and G-band carbon are at a proportion, determined using Raman spectroscopy to arrive at relative intensities of D-band carbon (ID) and G-band carbon (IG), such that a IG/ID ratio is in a range of 0 to about 2; (b) nitrogen at an amount, determined by X-ray photoelectron spectroscopy, that is in a range of about 0.3 atomic % to about 1.8 atomic % of the activated carbon particles, wherein at least some of the nitrogen atoms are substituted for carbon atoms in the crystal lattice structure of the G-band carbon sp2 hybridized graphitic phase; and (c) mesopores with diameters in a range of 2 nm to 5 nm and micropores with diameters less than 2 nm, the activated carbon particles having: (i) an average pore width, determined by the Barrett, Joyner, and Halenda (BJH) method, in a range of about 1 nm to about 4 nm; (ii) a microporous surface area, determined by the t-plot method, in a range of about 300 m2/g to about 1,350 m2/g; and (ii) a cumulative surface area of micropores with a hydraulic radius in a range of 0.285 nm to 1.30 nm that is in a range of about 1,000 m2/g to about 3,000 m2/g.