AU2012285404A1 - An energy storage device, an inorganic gelled electrolyte and methods thereof - Google Patents

An energy storage device, an inorganic gelled electrolyte and methods thereof Download PDF

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AU2012285404A1
AU2012285404A1 AU2012285404A AU2012285404A AU2012285404A1 AU 2012285404 A1 AU2012285404 A1 AU 2012285404A1 AU 2012285404 A AU2012285404 A AU 2012285404A AU 2012285404 A AU2012285404 A AU 2012285404A AU 2012285404 A1 AU2012285404 A1 AU 2012285404A1
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energy storage
storage device
electrolyte
energy
substrate
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AU2012285404A
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Anjan Banerjee
Shaik Abdul Gaffoor
Musuwathi Krishnamoorthy Ravikumar
Ashok Kumar Shukla
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Indian Institute of Science IISC
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Indian Institute of Science IISC
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/54—Electrolytes
    • H01G11/56—Solid electrolytes, e.g. gels; Additives therein
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/04—Hybrid capacitors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/46—Metal oxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/66—Current collectors
    • H01G11/68—Current collectors characterised by their material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/02—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 using combined reduction-oxidation reactions, e.g. redox arrangement or solion
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
    • H01G11/66—Current collectors
    • H01G11/70—Current collectors characterised by their structure
    • 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

Abstract

The present invention is related to hybrid capacitors specifically to PbO

Description

WO 2013/011464 PCT/IB2012/053658 "AN ENERGY STORAGE DEVICE, AN INORGANIC GELLED ELECTROLYTE AND METHODS THEREOF" TECHNICAL FIELD 5 The present disclosure is related to hybrid capacitors, specifically to PbO 2 /Activated Carbon hybrid ultracapacitors with an inorganic thixotropic-gelled-polymeric-electrolyte. The hybrid ultracapacitor of the present disclosure is simple to assemble, bereft of impurities and can be charged / discharged -rapidly- with high faradaic efficiency. 10 BACKGROUND OF THE INVENTION Supercapacitors (also termed as ultracapacitors) are being projected as devices that could enable major advances in energy storage. Supercapacitors are governed by the same physics as conventional capacitors, but utilize high-surface-area electrodes and thinner dielectrics to achieve greater capacitances, allowing energy densities greater than those of conventional 15 capacitors and power densities greater than those of batteries. Supercapacitors can be divided into three general classes, namely, electrical-double-layer capacitors, pseudocapacitors and hybrid capacitors. Each class is characterized by its unique mechanism for charge storage, namely faradaic, non-faradaic, and the combination of the two. Faradaic processes, such as oxidation-reduction reactions, involve the transfer of charge between electrode and electrolyte as 20 in a battery electrode, while a non-faradaic mechanism does not use a chemical mechanism rather, charges are distributed on surfaces by physical processes that do not involve the making or braking of chemical bonds similar to "the electrical double-layer". A hybrid supercapacitor combines a battery electrode where the energy is stored in chemical form, and an electrical double-layer electrode where the energy is stored in physical form. A PbO 2 /Activated Carbon 25 supercapacitor comprises a positive plate akin to a lead acid cell and a high surface-area activated carbon electrode as negative plate. The charge-discharge reactions at the positive and negative plates of such a hybrid supercapacitors are as follows. (+) plate: PbSO 4 +2H 2 0<-+PbO 2 + H 2 SO4 + 2H+ + 2e (-) plate: 2C + 2H+2e-<-+2(C-Hadsa)d 30 Accordingly, the net charge-discharge reactions for the hybrid supercapacitor can be written as WO 2013/011464 PCT/IB2012/053658 2 follows. PbSO 4 +2H 2 0+2C<-+PbO 2 + H2SO4+2(C-Hads)dl The (+) plate is realized by electrochemical formation and subsequent cycling in sulfuric acid / perchloric acid, while the (-) plate is prepared by pasting activated carbon onto a graphite 5 sheet. The said hybrid supercapacitor stores energy both in chemical and physical forms. The hybrid capacitors known in the prior art employ conventional PbO 2 plates that require sizing and mixing of the active materials of appropriate compositions, pasting, drying, curing and formation. Such electrodes are not fully amenable to fast charge/discharge processes desired in a capacitor. 10 STATEMENT OF THE INVENTION Accordingly, the present disclosure relates to an energy storage device (1), as shown in figure 1, comprising: a) substrate-integrated-lead-dioxide electrode (2), b) an activated carbon electrode (3), and c) a thixotropic inorganic-gel-polymer electrolyte (4) intercepted between the substrate 15 integrated-lead-dioxide electrode and the carbon electrode; an energy storage unit comprising plurality of energy storage device (1) as mentioned above, connected in series; a method of manufacturing an energy storage device (1), said method comprising acts of: a) preparing substrate-integrated lead dioxide electrode (2), b) preparing activated carbon electrode (3), and c) mounting the substrate-integrated lead dioxide electrode (2), the activated carbon electrode (3) 20 with a thixotropic inorganic-gel-polymer electrolyte (4) in between the substrate-integrated lead dioxide and the carbon electrode to manufacture the energy storage device; a method of using energy-storage device (1) or energy storage unit as mentioned above, said method comprising act of conjugating said energy-storage device or unit with electrical device for generating electrical energy to supply energy to devices in need thereof; and an inorganic thixotropic-gelled-polymer 25 electrolyte. BRIEF DESCRIPTION OF THE ACCOMPANYING FIGURES Figure 1 shows schematic diagram of a cell [energy storage device (1)] from the 12V substrate integrated PbO 2 /activated-carbon ultracapacitor with inorganic thixotropic-gelled-electrolyte.
WO 2013/011464 PCT/IB2012/053658 3 DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an energy storage device (1) comprising: a) a substrate-integrated-lead-dioxide electrode (2), 5 b) an activated carbon electrode (3), and c) a thixotropic inorganic-gel-polymer electrolyte (4) intercepted between the substrate- integrated-lead-dioxide electrode. In an embodiment of the present disclosure, the energy storage device (1) is a hybrid capacitor. In another embodiment of the present invention, the electrolyte acts as a separator. 10 In yet another embodiment of the present invention, the electrolyte is selected from a group comprising sulfuric acid, methanesulfonic acid and perflourosulfonic acid, preferably sulfuric acid. In yet another embodiment of the present invention,, the electrolyte is a thixtropic-gel obtained by cross-linking silica with sulfuric acid. 15 In still another embodiment of the present disclosure, the sulfuric acid has concentration ranging from about 4M to about 7M, preferably about 6M. In still another embodiment of the present disclosure, the energy storage device (1) is of faradaic efficiency ranging from about 88% to about 90%, preferably about 89%. The present disclosure relates to an energy storage unit comprising plurality of energy storage 20 device (1) as mentioned above, connected in series. The present disclosure relates to a method of manufacturing an energy storage device (1), said method comprising acts of: a) preparing substrate-integrated lead dioxide electrode (2), b) preparing activated carbon electrode (3), and 25 c) mounting the substrate-integrated lead dioxide electrode (2), the activated carbon electrode (3) with a thixotropic inorganic-gel-polymer electrolyte (4) in between the substrate-integrated lead dioxide and the carbon electrode to manufacture the energy storage device. In another embodiment of the present invention, the electrolyte acts as a separator. 30 The present invention relates to a method of using energy-storage device (1) or energy storage unit as mentioned above, said method comprising act of conjugating said energy-storage device WO 2013/011464 PCT/IB2012/053658 4 or unit with electrical device for generating electrical energy to supply energy to devices in need thereof. The present invention relates to an inorganic thixotropic-gelled-polymer-electrolyte. In an embodiment of the present invention, the electrolyte is prepared by cross-linking fumed 5 silica with sulfuric acid. In another embodiment of the present invention, the sulfuric acid has concentration ranging from about 4M to about 7M, preferably about 6M.; and wherein the electrolyte is capable of acting as a separator between electrodes of an energy storing device. 10 The present invention is related to realizing substrate-integrated PbO 2 /Activated-carbon hybrid ultracapacitor bereft of impurities. The hybrid ultra capacitors of the present invention are simple to assemble, bereft of impurities, and can be charged / discharged rapidly with faradaic efficiencies as high as 89%. 15 In the current invention, the positive electrodes, namely substrate-integrated PbO 2 , are made by electrochemical formation of pre-polished and etched lead metal sheets. Specifically, the substrate-integrated PbO 2 is obtained by oxidizing PbSO 4 which is formed when lead sheets come in contact with sulfuric acid. Subsequent to their formation, the electrodes are washed copiously with de-ionized water to wash off all the impurities. 20 Generally, electrodes in batteries are charged at C/10 rate (10h duration) and discharged at C/5 rate (5h duration). If the battery electrodes are charged/discharged at the rate C (1 hour) or at higher rates, their cycle-life is affected. Faradaic efficiency of the battery electrodes depends on the particle size of the active materials, porosity of the electrode, internal resistance of the 25 electrode, etc. The battery electrodes have low faradaic efficiency. The present invention provides electrochemically formed and substrate-integrated PbO 2 as battery-type electrode, which can be charged and discharged at higher rates, while retaining faradaic efficiencies as high as 89% with thixotropic gelled polymeric electrolyte. 30 The capacitance is calculated from the discharge curve using the equation: C(F) = I(A) x t(s)/(V 2
-VI)
WO 2013/011464 PCT/IB2012/053658 5 where V 2 is the voltage at the beginning of discharge and V1 is the voltage at the end of discharge. Pulsed cycle-life test involves the following four steps. 5 Step 1. Charging the ultracapacitor at 3A for 1 s. Step 2. Open-circuit voltage measurement for 5s. Step 3. Discharge the ultracapacitor at constant current at 3A. Step 4. Open-circuit voltage measurement for 5s. 10 The hybrid capacitor of the present invention is connected in series to obtain capacitors wherein the cell voltage gets added up, while the effective capacitance decreases, akin to conventional capacitor. 15 The method of manufacturing substrate-integrated PbO 2 /activated-carbon hybrid ultracapacitor (1) essentially comprises: preparing substrate-integrated lead dioxide electrode (2), preparing activated-carbon electrode (3), and mounting the substrate-integrated-lead-dioxide electrode (2), the activated-carbon electrode (3) with an inorganic thixotropic-gelled-polymeric-electrolyte (4) in between the substrate-integrated lead dioxide and the carbon electrode to manufacture the 20 energy-storage device. The present invention discloses substrate-integrated PbO 2 /activated-carbon hybrid ultracapacitors(HUC) with an inorganic thixotropic-gelled-polymer-electrolyte, which also acts as a separator. The gelled separator herein enhances the overall performance of the HUC with 25 respect to critical parameters, such as capacitance and cycle-life. The devices of the present invention can be easily conjugated with electrical devices for generating electrical energy as supply energy to devices in need thereof. 30 The technology of the instant invention is elaborated in detail with the help of following examples. However, the examples should not be construed as limiting the scope of the invention.
WO 2013/011464 PCT/IB2012/053658 6 Example: Preparation of substrate-integrated PbO 2 /Activated Carbon Hybrid Ultracapacitors A. Preparation of Substrate-Integrated PbO 2 Electrodes. Substrate-integrated- PbO 2 electrodes are prepared by etching pre-polished lead sheets (thickness 5 approximately 300 ptm) in IM HNO 3 for 60s and subsequently washed copiously with deionized water. The sheets were then immersed in 6 M aqueous H 2
SO
4 with 0.1 M HClO 4 as additive at room temperature. On immersing in aqueous sulfuric acid, a thin layer of lead sulfate is formed on the surface of the lead sheet which is oxidized to PbO 2 by using it as anode in an electrochemical cell fitted with a counter electrode. The process is repeated about five times to 10 prepare the fully-formed substrate-integrated PbO 2 electrodes. B. Preparation of PVDF bonded activated carbon electrodes. Activated-carbon electrodes are prepared by pasting activated carbon ink containing polyvinylidene difluoride (PVDF) as a binder. In brief, a carbon paste was obtained by mixing 85 wt.% of high-surface-area carbon (BET surface area is about 2000 m 2 /g and particle size of 15 about 10 ptm) with 10 wt. % of carbon black (particle size = 1 I pm) and 5 wt. % of binder like PVDF dissolved in an appropriate quantity of dimethylformamide solvent or Teflon (PTFE, poly-tetrafluoroethylene). Typically, 0.1 g of PVDF is dissolved in 10 ml of DMF and 1.7 g of high surface area carbon (Meadwestvaco product No. 090177) and 0.2 g of carbon black was added. The mixture was mixed well in an ultrasonicator for 5 min. The resulting carbon ink was 20 brush coated onto two graphite electrodes of area 4.5 cm x 7 cm, which had a tag area of 0.5 cm width and 0.5 cm length. The carbon paste was applied on both sides of the carbon electrodes so that each side of the electrode in order to get a 0.5 g of active material. Then the electrodes were dried in air oven for overnight (about 10 h) at 80 0 C. C. Assembly of 12V Substrate-Integrated PbO 2 -AC Hybrid Ultracapacitors (HUCs) 25 A 12V substrate-integrated PbO 2 /Activated carbon hybrid ultracapacitor was realized by connecting six single cells in series in a commercial lead-acid battery container. Each cell of this 12V hybrid ultracapacitor comprises 9 positive and 8 negative plates, each of size 4.5 cm x 7 cm, with the tag area of 0.5cm x 0.5 cm and 0.3 mm thickness for the positive plate and 0.8 mm WO 2013/011464 PCT/IB2012/053658 7 thickness for negative plates. An inorganic thixotropic-gelled-polymer-electrolyte that was also used as a separator was prepared by cross-linking fumed silica with 6 M sulfuric acid. A unique method was used to interconnect the graphite electrodes. The tag portion of the negative electrodes is electroplated with tin, followed by electroplating with lead, which facilitates the 5 graphite electrode tags to be soldered to each other. The graphite electrodes in each cell were soldered with lead by torch-melt method using an appropriately designed group-burning fixture. Subsequently, the cells were interconnected in series. The gelled electrolyte separator used herein enhances the overall performance of the HUC with respect to critical parameters such as cycle-life and capacitance. The comparative data for the 10 12V Absorbent Glass-Mat (AGM)-HUC and 12 V Gelled-HUC are given in Table 1 below. AGM-HUC Gelled-HUC Internal Resistance 90 m ohm 120 m ohm Faradaic Efficiency 91% 89% Capacitance 300mA 184 F 269 F 600mA 163 F 255 F 900mA 150 F 239 F 1.2A 138 F 222 F 1.5A 130 F 208 F Leakage Current after 15 mA 35 mA 24h Self Discharge after 130% 16 % 24 h Table 1: Comparison between AGM-HUC and Gelled-HUC. While various aspects and embodiments of the present invention have been disclosed herein, 15 other aspects and embodiments will be apparent to those skilled in the art. The various aspects and embodiments disclosed herein are for purposes of illustration and are not intended to be limiting, with the true scope and spirit being indicated by the following claims.

Claims (14)

1. An energy storage device (1) comprising: a) a substrate-integrated-lead-dioxide electrode (2), b) an activated carbon electrode (3), and 5 c) a thixotropic inorganic-gel-polymer electrolyte (4) intercepted between the substrate- integrated-lead-dioxide electrode and the carbon electrode.
2. The energy storage device as claimed in claim 1, wherein the energy storage device (1) is a hybrid capacitor.
3. The energy storage device as claimed in claim 1, wherein the electrolyte acts as a 10 separator.
4. The energy storage device as claimed in claim 1, wherein the electrolyte is selected from a group comprising sulfuric acid, methanesulfonic acid and perflourosulfonic acid, preferably sulfuric acid.
5. The energy storage device as claimed in claim 4, wherein the electrolyte is a thixotropic 15 gel obtained by cross-linking silica with sulfuric acid.
6. The energy storage device as claimed in claim 4, wherein the sulfuric acid has concentration ranging from about 4M to about 7M, preferably about 6M.
7. The energy storage device as claimed in claim 1, wherein the energy storage device (1) is of faradaic efficiency ranging from about 88% to about 90%, preferably about 89%. 20
8. An energy storage unit comprising plurality of energy storage device (1) of claim 1 connected in series.
9. A method of manufacturing an energy storage device (1), comprising acts of: a) preparing substrate-integrated lead dioxide electrode (2), b) preparing activated carbon electrode (3), and 25 c) mounting the substrate-integrated lead dioxide electrode (2), the activated carbon electrode (3) with a thixotropic inorganic-gel-polymer electrolyte (4) in between the substrate-integrated lead dioxide and the carbon electrode to manufacture the energy storage device.
10. The method as claimed in claim 9, wherein the electrolyte acts as a separator. 30
11. A method of using energy-storage device (1) as claimed in claim 1 or energy storage unit as claimed in claim 7, said method comprising act of conjugating said energy-storage WO 2013/011464 PCT/IB2012/053658 9 device or unit with electrical device for generating electrical energy to supply energy to devices in need thereof.
12. An inorganic thixotropic-gelled-polymer-electrolyte.
13. The electrolyte as claimed in claim 12, wherein the electrolyte is prepared by cross 5 linking fumed silica with sulfuric acid.
14. The electrolyte as claimed in claim 13, wherein the sulfuric acid has concentration ranging from about 4M to about 7M, preferably about 6M.; and wherein the electrolyte is capable of acting as a separator between electrodes of an energy storing device.
AU2012285404A 2011-07-18 2012-07-18 An energy storage device, an inorganic gelled electrolyte and methods thereof Abandoned AU2012285404A1 (en)

Applications Claiming Priority (3)

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IN2441/CHE/2011 2011-07-18
IN2441CH2011 2011-07-18
PCT/IB2012/053658 WO2013011464A1 (en) 2011-07-18 2012-07-18 An energy storage device, an inorganic gelled electrolyte and methods thereof

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CN108493500B (en) * 2018-04-26 2020-05-29 包头昊明稀土新电源科技有限公司 Capacitive nickel-hydrogen power battery and preparation method thereof
CN110208996B (en) * 2019-07-08 2021-01-22 上海大学 Gel electrolyte and preparation method and application thereof
CN113506683B (en) * 2020-06-12 2022-09-13 吉林大学 Lead-carbon supercapacitor cathode and preparation method thereof

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KR101050021B1 (en) * 2006-10-23 2011-07-19 액시온 파워 인터네셔널, 인크. Cathode for Hybrid Energy Storage Devices
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WO2010151227A1 (en) * 2009-06-26 2010-12-29 Nanyang Technological University Energy charge storage device using a printable polyelectrolyte as electrolyte material
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JP2014521231A (en) 2014-08-25
ZA201400288B (en) 2014-10-29
WO2013011464A1 (en) 2013-01-24
BR112014001141A2 (en) 2017-02-21
KR20140043788A (en) 2014-04-10
EP2735008A1 (en) 2014-05-28
CN103875050A (en) 2014-06-18

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