Patent Description:
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.

As alternative energy, renewable energy and electric cars grow more and more popular, existing energy storage technology is inadequate and will continue to fall short of meeting the growing demand for absorbing, storing and rapidly delivering of electrical energy unless a new energy storage solution is found. A major focus has been on lithium-based chemistry for rechargeable batteries. These batteries involve chemical reactions to store electric power. The reactions are slow and generate heat, which causes inherent loss of energy. In most battery embodiments, one electrode has significant carbon makeup. The other electrode's potency is a function of its surface area and pore volume that therein provides molecular sites for the electrochemical reaction and hence for electric charge energy storage to occur.

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.

These 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.

Although 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.

<NPL>, discloses various methods for chemical activation of a biochar structure.

A need exists for systems/methods that overcome the inherent trade-off between storage capacity and discharge rate, as discussed above.

The present invention provides a method according to claim <NUM> comprising applying an electrochemical treatment of electrolysis to monolithic carbonaceous biochar electrodes made from monolithic biochar wafers.

Embodiments of the invention are set forth with the appended dependent claims.

The present disclosure provides an advantageous electrolysis treatment pursuant to which, in an aqueous (water) electrolyte bath condition, water (H<NUM>O) is split at the outer and inner surfaces of the pores in the electrode to form hydrogen (H<NUM>) gas and oxygen (O<NUM>) 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.

Furthermore, the ambiance of water electrolysis which produces the hydrogen, oxygen, and related solute molecular species (H<NUM>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. Furthermore, 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.

Additionally, 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.

Additional features, functions and benefits of the disclosed systems and methods will be apparent from the description which follows.

To assist those of ordinary skill in the art in making and using the disclosed systems/methods, reference is made to the accompanying figures, wherein:.

With reference to the exemplary setup schematically depicted in <FIG>, the following components are identified as:.

With reference to the exemplary setup schematically depicted in <FIG>, the following components are identified as:
<NUM>: Overall apparatus setup for implementation of the disclosed methods for multiple pairs of electrodes (<NUM>), (<NUM>) being treated by Electro-Activation, each fastener clip being larger or longer than shown in <FIG> so as to hold more than one electrode of each polarity, with the limitation that only one fastener clip of each polarity "A", "B" is used.

With reference to the exemplary setup schematically depicted in <FIG>, the following components are identified as:
<NUM>: Overall apparatus setup for implementation of the disclosed methods for multiple pairs of electrodes being treated by Electro-Activation, each fastener clip being larger or longer than shown in <FIG> 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.

With reference to the flowchart schematically depicted in <FIG> and <FIG>, these figures show Scanning Electron Microscopy (herein after SEM) images of two similar electrodes, each being treated for activation by different methods disclosed herein.

<NUM>: 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 <NUM> shows the disclosed Carbonaceous Biochar Monolithic Wafers (<NUM>).

<NUM>: SEM image of the results of a Monolithic Carbonaceous Biochar Electrode material having been activated by common Steam-Carbon reaction having been treated in the High Temperature Furnace with the optional Steam-Activation step.

<NUM>: A graphical annotation highlighting the SEM screen image (<NUM>) showing a relative scale related to the screen image for a length dimension of <NUM> microns.

<NUM>: A datum from the SEM indicating on the SEM screen image (<NUM>) the magnification of the image of <NUM>,<NUM> times.

<NUM>: Reference <NUM> shows an SEM image of the disclosed Carbonaceous Biochar Monolithic Wafer (<NUM>). 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.

<NUM>: 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 <NUM> are evident versus <NUM> 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.

Regarding <FIG>, 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.

<NUM>: The overall collection of four (<NUM>) SEM images depicting progressive magnification of the same area of the interior of an electrode treated by the Electrolysis-Activation method disclosed herein.

<NUM>: An SEM image of the inner structures of the pores and channels of the disclosed Monolithic Carbonaceous Biochar Electrode having been treated by the disclosed method, viewed at <NUM>,000x magnification. Further, a graphical delineation (black box and arrow) indicating the zoom area for further magnification that is subsequently shown in <NUM>. Further, a graphical delineation (black circle) highlighting the relative dimension of the SEM image on the SEM screen capture showing the reference length of <NUM> microns relative to the SEM screen image. Note that in image <NUM>, the preferential graphene and graphitic self-assembled platelets and structures only appear as a fuzzy surface on the image of the treated biochar.

<NUM>: An SEM image of the inner structures of the pores and channels of the disclosed Monolithic Carbonaceous Biochar Electrode having been treated by the disclosed method, viewed at <NUM>,000x magnification. Further, a graphical delineation (black box and arrow) indicating the zoom area for further magnification that is subsequently shown in <NUM>. Further, a graphical delineation (black circle) highlighting the relative dimension of the SEM image on the SEM screen capture showing the reference length of <NUM> micron relative to the SEM screen image. Note that in image <NUM>, the preferential graphene and graphitic self-assembled platelets and structures only appear as a fuzzy surface on the image of the treated biochar.

<NUM>: An SEM image of the inner structures of the pores and channels of the disclosed Monolithic Carbonaceous Biochar Electrode having been treated by the disclosed method, viewed at <NUM>,000x magnification. Further, a graphical delineation (black box and arrow) indicating the zoom area for further magnification that is subsequently shown in <NUM>. Further, a graphical delineation (black circle) highlighting the relative dimension of the SEM image on the SEM screen capture showing the reference length of <NUM> micron relative to the SEM screen image. Note that in image <NUM>, the preferential graphene and graphitic self-assembled platelets and structures are clearly visible in the SEM image and can be identified on the surface of the treated biochar.

<NUM>: An SEM image of the inner structures of the pores and channels of the disclosed Monolithic Carbonaceous Biochar Electrode having been treated by the disclosed method, viewed at <NUM>,740x magnification. Further, a graphical delineation (black circle) highlighting the relative dimension of the SEM image on the SEM screen capture showing the reference length of <NUM> nanometers relative to the SEM screen image. Note that in image <NUM>, the preferential graphene and graphitic self-assembled platelets and structures are clearly visible and obvious in the SEM image and can be identified on the surface of the treated biochar. Furthermore, the image demonstrates that the carbonaceous structures that have plated out of solution during implementation of the disclosed method are thin and flat or curved platelets of single layer and few layer graphene, having been additionally tested by the Elemental Analysis Feature of the SEM system.

<NUM>: Reference for two SEM images (<NUM>) and (<NUM>) side by side of the same area of the untreated Monolithic Carbonaceous Biochar Electrode under different magnification.

<NUM>: An SEM image of the untreated the surface, pores and channels of the carbonaceous biochar material at magnification of 500x.

<NUM>: A graphical delineation (black circle) of the SEM screen image showing the dimension length relative to the screen image of <NUM> microns.

<NUM>: An SEM image of the untreated surface, pores and channels of the carbonaceous biochar material at magnification of <NUM>,000x.

<NUM>: A graphical delineation (black circle) of the SEM screen image showing the dimension length relative to the screen image of <NUM> micron.

<NUM>: Reference for two SEM images (<NUM>) and (<NUM>) side by side of the same area of the treated Monolithic Carbonaceous Biochar Electrode under different magnification.

<NUM>: An SEM image of the preferentially grown and self-assembled iron flake and flower petal-like structures covering the surface, pores and channels of the carbonaceous biochar material.

<NUM>: A graphical delineation (black box) of the SEM screen image showing the magnification of <NUM>,000x.

<NUM>: An SEM image of the preferentially grown and self-assembled iron flake and flower petal-like structures covering the surface, pores and channels of the carbonaceous biochar material at higher magnification than (<NUM>).

Claim 1:
A method comprising:
applying an electrochemical treatment of electrolysis to monolithic carbonaceous biochar electrodes (<NUM>,<NUM>) made from monolithic biochar wafers (<NUM>);
wherein said monolithic carbonaceous biochar electrodes comprise surfaces, channels and pores, said pores including pore surfaces, and
wherein one or more organic moieties reside within the pores, at the pore surfaces or are chemically bound to the carbonaceous structures of the carbonaceous biochar electrodes;
wherein the applied electric potential is effective to cause the electrolysis of water of the aqueous electrolyte salt bath;
wherein applying said electrochemical treatment of electrolysis modifies desired properties of the monolithic biochar wafers;
wherein an applied electric potential greater than <NUM> V is used to activate said monolithic carbonaceous biochar electrodes made from biochar wafers clamped to current conducting fasteners, and said biochar wafers are submerged into an aqueous electrolyte salt bath, and
characterized in that the applied electric voltage polarity of the electrodes is cycled every <NUM> to <NUM> minutes per polarity for a total of <NUM> to <NUM> cycles.