US20200350553A1 - Process for Producing Highly Activated Electrode Through Electro-Activation - Google Patents

Process for Producing Highly Activated Electrode Through Electro-Activation Download PDF

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Publication number
US20200350553A1
US20200350553A1 US16/935,850 US202016935850A US2020350553A1 US 20200350553 A1 US20200350553 A1 US 20200350553A1 US 202016935850 A US202016935850 A US 202016935850A US 2020350553 A1 US2020350553 A1 US 2020350553A1
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Prior art keywords
electrode
biochar
electrodes
pores
carbonaceous
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Abandoned
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US16/935,850
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English (en)
Inventor
Dino Favetta
Tao Chen
Eric P. Boon
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Controlamatics Corp
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Controlamatics Corp
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Priority to US16/935,850 priority Critical patent/US20200350553A1/en
Assigned to CONTROLAMATICS CORPORATION reassignment CONTROLAMATICS CORPORATION ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: CHEN, TAO, BOON, Eric P., Favetta, Dino
Publication of US20200350553A1 publication Critical patent/US20200350553A1/en
Priority to US17/854,790 priority patent/US20220336786A1/en
Abandoned legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00—Electroplating characterised by the article coated
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/44—Raw materials therefor, e.g. resins or coal
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0438—Processes of manufacture in general by electrochemical processing
    • H01M4/045—Electrochemical coating; Electrochemical impregnation
    • H01M4/0452—Electrochemical coating; Electrochemical impregnation from solutions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/133—Electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8803—Supports for the deposition of the catalytic active composition
    • H01M4/8807—Gas diffusion layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • H01M4/8853—Electrodeposition
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/90—Selection of catalytic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/96—Carbon-based electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present disclosure describes a method of treatment of an electrode material with an applied electrical potential and electric current, to induce electrolysis treatment of the electrode.
  • Ultra-capacitors store electrical energy by an electrostatic mechanism, not a chemical reaction as found in batteries. Therefore, the electric charge storage mechanism in ultra-capacitors is not rate-limited by a chemical reaction.
  • the superior charge storage capability of ultra-capacitors is a function of pore volume and surface area.
  • the energy storage mechanism of ultra-capacitors via transport of ions and attraction to the charge storage sites on the electrodes is limited in the existing technology because of the electrode morphology applied to the supporting members (foils, membranes, separators, etc.) that form “packaging overhead” in the overall ultra-capacitor device assembly for the given amount of electrode material.
  • Limitations of that electrode layer in existing ultra-capacitor technology are founded in either the thickness of the electrode as it resides between the charge collector metal foil and the non-conductive separator membrane, as well and the total surface area within the channels, walls and pores of the electrode.
  • Electrodes are generally fabricated from electrically conductive activated carbon.
  • Other materials for the electrode apply highly scientific and costly engineered materials such as carbon nanotubes, fullerenes, “Bucky-Balls” and other such mesh-like and web-like molecular structures, to increase the available surface area within the pores, walls and channels of the electrode.
  • ultra-capacitors store much more electric energy than standard capacitors, they generally store orders of magnitude less electric energy than lithium-based batteries. Since there is no chemical reaction in ultracapacitors as found in batteries, ultra-capacitors charge and discharge their energy orders of magnitude faster than batteries. According to conventional technologies, the electrical storage performance comparison between batteries and ultracapacitors becomes a trade-off.
  • the present disclosure provides an advantageous electrolysis treatment pursuant to which, in an aqueous (water) electrolyte bath condition, water (H 2 O) is split at the outer and inner surfaces of the pores in the electrode to form hydrogen (H 2 ) gas and oxygen (O 2 ) gas that escape out of the carbonaceous electrode pores into the bath and expel loose materials (carbonaceous and other impurities) from inside the electrode pores outward.
  • This outward escape of gas serves as a pore generation and pore expansion treatment, thus initially activating or further activating the electrode.
  • the ambience of water electrolysis which produces the hydrogen, oxygen, and related solute molecular species (H 3 O + , H + , OH ⁇ , etc.) also kinetically react and electro-chemically react with materials of the carbonaceous electrodes, and remove undesirable compounds, thereby further activating the electrodes.
  • the kinetically driven reactions and electrochemically driven reactions can be selectively controlled to remove undesirable materials from the electrode and not affect or minimally affect the base carbon structures and materials of the electrode by control of the voltage window applied in the disclosed treatment.
  • these electrochemically driven and kinetically driven cleaning reactions can be controlled, enhanced and modified by addition of other solutes, salts, acids an bases in the electrolyte solution.
  • the disclosed electrolysis treatment of the carbonaceous electrode grows advantageous nanostructures that are electrodeposited plating material on the surface of the electrode and in the channels and pores of the electrode which increase the surface area and therefore increases the energy storage capability when the electrodes are used in an electric double layer capacitor, ultracapacitor, pseudo-capacitor, battery or fuel cell as electrodes, or as any other adsorbing or adsorbing-desorbing function, or as electrodes in water-electrolysis based hydrogen gas and oxygen gas generators.
  • FIGS. 1A thru 1 D schematically depict an exemplary electrochemical setup according to the present disclosure
  • FIGS. 2A-2B are SEM images of untreated versus treated carbonaceous biochar electrode wafers
  • FIG. 3 provides four (4) SEM images depicting progressive magnification of the same area of the interior of an electrode treated by the electrolysis-activation method disclosed herein;
  • FIG. 4 provides two (2) SEM images of the same area of an untreated monolithic carbonaceous biochar electrode under different magnification revealing the absence of preferential structures otherwise created by the disclosed method
  • FIG. 5 provides two (2) SEM images of the same area of the treated monolithic carbonaceous biochar electrode under different magnifications.
  • the DC Power Source hereinafter Power Supply (in an exemplary implementation, the DC Power Supply is a TekPower Model TP3005T DC Power Supply)
  • the stimulus can originate from within the Voltage Polarity Reversing Device ( 112 ) or be external to the Voltage Polarity Reversing Device ( 112 )
  • a Voltage Polarity Reversing Device such that two distinct states of Direct Output Polarity and Reverse Output Polarity are possible when observing or measuring the device ( 112 ) output polarity terminals “A” and “B” relative to the device input polarity, and such device having a polarity switching activation caused by mechanical electrical stimulus ( 111 ), such as a timing device, such as manual manipulation.
  • the output terminals of ( 112 ) are labeled A and B wherein, when the Voltage Polarity Reversing Device ( 112 ) is in the initial or resting state (unmanipulated by ( 111 ) or unstimulated by ( 111 )) the “A” terminal provides the Positive Voltage Potential and the “B” Terminal provides the Negative Voltage Potential sourced from the DC Powe Supply ( 105 ).
  • the Voltage Polarity Reversing Device ( 112 ) when the Voltage Polarity Reversing Device ( 112 ) is in the active state (manipulated by ( 111 ) or stimulated by ( 111 )) and device ( 112 ) performs its Voltage Polarity Reversing function the “B” terminal provides the Positive Voltage Potential and the “A” Terminal provides the Negative Voltage Potential as sourced by the DC Power Supply ( 105 ).
  • Electrolyte Bath Vessel made of non-electrically conductive material.
  • each fastener clip being larger or longer than shown in FIG. 1A so as to hold more than one electrode of each polarity, with the extension that a multiplicity fastener clips of each polarity is used, and wherein the arrangement of each parallel fastener clip is such that the assigned polarity alternates from one fastener clip rail to the next along the arrangement.
  • Electro-Activation Overall apparatus setup for implementation of the disclosed methods for a single pair of electrodes being treated by Electro-Activation, wherein the electrodes may be of significant size and weight such that the conductive fastener clips alone may not be sufficient to support and hold the electrodes submerged into the bath, thereby requiring an additional support ( 191 ).
  • Supports ( 191 ) An added support device of non-electrically conductive material providing mechanical support to the electrodes that are otherwise hanging from the conductive fastener clips, the addition of such supports ( 191 ) thereby preventing breakage of the electrodes due to gravimetric stress. Supports ( 191 ) are further connected to other external support devices (not shown) to assist in suspending the electrodes ( 150 ), ( 151 ) in the electrolyte bath ( 140 ).
  • FIGS. 2A and 2B show Scanning Electron Microscopy (herein after SEM) images of two similar electrodes, each being treated for activation by different methods disclosed herein.
  • Image 200 Overall depiction of the SEM Image therein showing a magnified image of the surface and inner body of a Monolithic Carbonaceous Biochar Electrode material resulting from treatments disclosed herein.
  • Image 200 shows the disclosed Carbonaceous Biochar Monolithic Wafers ( 210 ).
  • Reference 250 shows an SEM image of the disclosed Carbonaceous Biochar Monolithic Wafer ( 260 ).
  • the overall depiction of the SEM Image therein shows a magnified image of the surface and inner body of the Monolithic Carbonaceous Biochar Electrode material resulting from treatments disclosed in this embodiment.
  • 260 SEM image of the results of a Monolithic Carbonaceous Biochar Electrode material having been activated by the disclosed Electrolysis-Activation step. A distinct “Fuzzines” of the surfaces of 260 are evident versus 210 which shows no “Fuzziness”, such observable “fuzziness” being the growth of preferential nano- and micro-structures of carbon, specifically graphene and graphitic structures plated onto the monolithic biochar pore surfaces due to treatments by the disclosed methods.
  • an electrolyzed carbonaceous monolithic biochar wafer electrode is provided showing growth of preferential graphene and graphitic structures for superior surface area improvement for dramatic increase in capacitance. These graphene and graphitic structures are caused by the treatments to the biochar due to the disclosed method.
  • the same treated electrodes exhibit over 150 Farads/gram and up to 300 Farads/gram when used in an ultra-capacitor.
  • porous non-conducting separators can include a simple sponge or open-cell polymer foam rubber, porous plastic film, woven or non-woven cloth of polymer fiber, ceramic fiber, or silica-based fibers such as glass wool insulation and the like.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Power Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Inert Electrodes (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Water Treatment By Electricity Or Magnetism (AREA)
US16/935,850 2019-03-29 2020-07-22 Process for Producing Highly Activated Electrode Through Electro-Activation Abandoned US20200350553A1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US16/935,850 US20200350553A1 (en) 2019-03-29 2020-07-22 Process for Producing Highly Activated Electrode Through Electro-Activation
US17/854,790 US20220336786A1 (en) 2019-03-29 2022-06-30 Process for Producing Highly Activated Electrode Through Electro-Activation

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US201962826038P 2019-03-29 2019-03-29
PCT/US2020/025648 WO2020205697A1 (fr) 2019-03-29 2020-03-30 Procédé de production d'une électrode hautement activée par électro-activation
US16/935,850 US20200350553A1 (en) 2019-03-29 2020-07-22 Process for Producing Highly Activated Electrode Through Electro-Activation

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EP (1) EP3947782A4 (fr)
JP (1) JP7441855B2 (fr)
KR (1) KR20210145219A (fr)
CN (1) CN113892158B (fr)
AU (1) AU2020256132A1 (fr)
CA (1) CA3135353A1 (fr)
EA (1) EA202192594A1 (fr)
MX (1) MX2021011890A (fr)
WO (1) WO2020205697A1 (fr)
ZA (1) ZA202108298B (fr)

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CN113387416B (zh) * 2021-04-20 2023-02-24 云南华谱量子材料有限公司 一种石墨烯复合光催化玻璃纤维电极材料及其制备方法
KR20240088054A (ko) 2022-12-13 2024-06-20 전북대학교산학협력단 바이오차의 전기화학적 개질 방법

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JPH09129515A (ja) * 1995-11-01 1997-05-16 Isuzu Motors Ltd 電気二重層コンデンサおよびその電極の製造方法
JP3973183B2 (ja) 1998-09-22 2007-09-12 株式会社パワーシステム 電気二重層コンデンサの製造方法
CN101302051B (zh) * 2008-01-22 2011-11-23 南京大学 一种用于含酚废水电化学处理的石墨电极
KR20110080393A (ko) 2010-01-05 2011-07-13 삼성전자주식회사 전기 흡착 탈이온 장치용 전극의 제조방법, 전기 흡착 탈이온 장치용 전극 및 상기 전극을 구비하는 전기 흡착 탈이온 장치
JP5846575B2 (ja) 2011-09-16 2016-01-20 国立大学法人九州工業大学 電気二重層キャパシタの製造方法
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US20220336786A1 (en) 2022-10-20
MX2021011890A (es) 2021-12-15
WO2020205697A1 (fr) 2020-10-08
KR20210145219A (ko) 2021-12-01
CN113892158A (zh) 2022-01-04
EP3947782A4 (fr) 2023-01-25
CA3135353A1 (fr) 2020-10-08
AU2020256132A1 (en) 2021-11-04
JP2022526441A (ja) 2022-05-24
ZA202108298B (en) 2023-01-25
CN113892158B (zh) 2024-08-20
JP7441855B2 (ja) 2024-03-01
EA202192594A1 (ru) 2022-03-24
EP3947782A1 (fr) 2022-02-09

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