WO2014151372A1 - Graphene / carbon compositions - Google Patents

Graphene / carbon compositions Download PDF

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Publication number
WO2014151372A1
WO2014151372A1 PCT/US2014/025594 US2014025594W WO2014151372A1 WO 2014151372 A1 WO2014151372 A1 WO 2014151372A1 US 2014025594 W US2014025594 W US 2014025594W WO 2014151372 A1 WO2014151372 A1 WO 2014151372A1
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Prior art keywords
carbon
graphene
activated carbon
nanosized
nano sized
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Ceased
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PCT/US2014/025594
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French (fr)
Inventor
Inhwan Do
Hyunjoong Kim
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Priority to EP14769687.6A priority Critical patent/EP2973805A4/en
Priority to KR1020157029176A priority patent/KR20150132394A/en
Priority to JP2016501889A priority patent/JP2016518705A/en
Priority to CN201480022773.8A priority patent/CN105122520A/en
Publication of WO2014151372A1 publication Critical patent/WO2014151372A1/en
Anticipated expiration legal-status Critical
Ceased 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
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • 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
    • H01G11/38—Carbon pastes or blends; Binders or additives therein
    • 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

Definitions

  • the instant invention deals with new compositions of matter.
  • the invention uses high surface area nano sized graphene and carbon for capacitors.
  • Activated carbons are materials commonly used in commercial electrochemical capacitors. However, they do not deliver sufficient performance necessary for applications requiring high energy and power density. This lack of performance is due to poor electrical conductivity and poorion transport caused by very wide size distributions of randomly interconnected inner micropores.
  • Nano sized graphene is used in electrochemical capacitors due to its high surface area, high mechanical and electrical properties, highly inert surface properties, low impurities, and the like. Nano sized graphene consists mostly of mesopores and macropores and thus the surface area of the nano sized graphene is accessible by even fairly large electrolyte ions. The nano sized graphene with surface areas of 600 mVg shows very high specific capacitance outperforming the new carbon
  • nanostriictures such as singl walled and double wailed carbon nanotubes having comparable surface areas to nano sized
  • the graphene reduces the cost of the electrode by replacing high cost activated carbon with lower cost graphene while improving energy storage by at least 5 to 20%.
  • the graphene also acts as an ion migration catalyst to increase both energy and power density * Internal resistance is also reduced.
  • auxiliar agent that may be carbon black.
  • embodiment is a composition of matter comprising a combination of a high surface area nano sized graphite, and carbon.
  • the graphites are nanosized graphene nanotu ' bes and anosized
  • graphene nanoplatelets and the carbons can be, for example, activated carbon, carbon black, and carbon nanofibers and carbon aerogels.
  • a method for manufacturing a composition as set forth Supra comprises dispersing graphene in a suitable- solvent,, dispersing carbon in a suitable solven f combining and mixing the products together to form a slurry,, filtering the slurry to provide a sheet form, drying the sheet f and ,
  • Figure 1 is a chart of Galvariostatic charge/discharge for the electrochemical characterisation of the material prepared in example 1 with gravimetric capacitance in F/g (faraday/gram) versus current density in A/g (amps/gram) »
  • Figure 2 is a chart of volumetric capacitance with Current Density in A/g versus Volumetric Capacitance in F/cm 3' .
  • Figure 3 is a chart of gravimetric energy in j3 ⁇ 4h/kg versus
  • Figure 4 is a chart of Volumetric Energy in m h/cn versus Current Density in A/g
  • Figure 5 is a chart of Gravimetric Power in kW/kg versus Current Density in A/g.
  • Figure 6 is a chart of volumetric Power in W/'cm 3 versus Current density in A/g
  • the instant invention deals with the addition of graphene into activated carbon,
  • the carbon useful herein has an average size of between 10. nanometer and 100 microns and a BET surface area greater than about 300 m 2 /g.
  • the graphene has a size between 30 nanometers and 50 microns and a BET surface of greater than about 300 mVg.
  • the graphene has an aspect ratio between about 25 and 25,000.
  • the graphene to carbon ratio is between 0,5 and 10.
  • 1 designates 100% YP50F 2 designates 90% YP50F and 10% C7-5.0; 3 designates 80% YP50F and 20% C?50; 4 designates 70% YP50F and 30% C7S0; 5 designates 60% YP50F and 40% C750; 6 designates 50% YP50F and 50% C75Q, weight ratios.
  • YP-50F ISOQmVg, uraray Chemical Company
  • MSP-20 22QQHrVg, ansai Chemical Company.
  • Manosized graphene ⁇ C-750, 75QraVg)- and multi-walled carbon nanotubes ⁇ 23 . 0m 2 g, Ranwh
  • Nanotech were used as another active material and the binder, respectively.
  • Activated carbon or the activated carbon /nano sized graphene was dispersed in isopropyl alcohol using a bath type so icator for 60 minutes and carbon nano tubes was also separately sonicated in Isopropyl alcohol for 1 hour.
  • the dispersed activated carbon and the carbon nano tubes solutions were combined, followed by additional 60 minutes sonication. Then, the activated carbon-carbon nano tubes and activated carbon/nano sized graphene-carbon nanotubes dispersion (ink) was filtered using a membrane filtration system.

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Nanotechnology (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Organic Chemistry (AREA)

Abstract

High surface area nano sized grapheme and carbon compositions.

Description

GRAPHENE / CARBON COMPOSITIONS
We, Inhwan Do, residing in the City of East Lansing, Comity of Ingham, State of Michigan, a citizen of South Korea and Hyunjoong Kim, residing in the city of East
Lansing, County of Ingham, and State of Michigan, a citizen of South Korea, have invented new and novel compositions of matter which are
GRAPHENE / CARBON COMPOSITIONS
The following of which is a specification therefor.
This application claims priority from U.S. Provisional Patent application serial
number 61/786,735, filed March 15, 2013.
The instant invention deals with new compositions of matter.
The invention uses high surface area nano sized graphene and carbon for capacitors.
Graphene /Carbon hybrid electrodes exhibit synergic effects on the performance
enhancement of electrochemical capacitors. Both forms of activated carbon act as an active material and graphene acts as an active material,
Activated carbons are materials commonly used in commercial electrochemical capacitors. However, they do not deliver sufficient performance necessary for applications requiring high energy and power density. This lack of performance is due to poor electrical conductivity and poorion transport caused by very wide size distributions of randomly interconnected inner micropores.
Graphene is used in electrochemical capacitors due to its high surface area, high mechanical and electrical properties, highly inert surface properties, low impurities, and the like. Nano sized graphene consists mostly of mesopores and macropores and thus the surface area of the nano sized graphene is accessible by even fairly large electrolyte ions. The nano sized graphene with surface areas of 600 mVg shows very high specific capacitance outperforming the new carbon
nanostriictures such as singl walled and double wailed carbon nanotubes having comparable surface areas to nano sized
graphene .
The graphene reduces the cost of the electrode by replacing high cost activated carbon with lower cost graphene while improving energy storage by at least 5 to 20%. The graphene also acts as an ion migration catalyst to increase both energy and power density* Internal resistance is also reduced.
The process and materials of this invention are different from any found in the prior art » The only reference that calls directly for using carbon black and graphene in an electrode together does so only to increase the conduction with a metal based active material. It is not shown or suggested that the active material is a activated carbon enhanced with graphene.
Such a disclosure can be found in U.S. 2012/0088156A wherein the application teaches a multistep method to produce electrodes that includes adding graphene oxide to an electrode mixture and reducing the graphene oxide to graphene. One of the dependent claims includes adding less than 1% conductive
auxiliar agent that may be carbon black.
THE IIIVE53 ION
Thus, what is disclosed and claimed herein as one
" embodiment is a composition of matter comprising a combination of a high surface area nano sized graphite, and carbon. The graphites are nanosized graphene nanotu'bes and anosized
graphene nanoplatelets and the carbons can be, for example, activated carbon, carbon black, and carbon nanofibers and carbon aerogels.
? Also, there is present in this invention a method for manufacturing a composition as set forth Supra . The process of manufacturing comprises dispersing graphene in a suitable- solvent,, dispersing carbon in a suitable solven f combining and mixing the products together to form a slurry,, filtering the slurry to provide a sheet form, drying the sheetf and ,
calendaring the sheet to a desired thickness and surface finish,
BRIEF DESCRIPTION OF THE
Figure 1 is a chart of Galvariostatic charge/discharge for the electrochemical characterisation of the material prepared in example 1 with gravimetric capacitance in F/g (faraday/gram) versus current density in A/g (amps/gram) »
Figure 2 is a chart of volumetric capacitance with Current Density in A/g versus Volumetric Capacitance in F/cm3'.
Figure 3 is a chart of gravimetric energy in j¾h/kg versus
Current Density in A/g,
Figure 4 is a chart of Volumetric Energy in m h/cn versus Current Density in A/g,
Figure 5 is a chart of Gravimetric Power in kW/kg versus Current Density in A/g.
Figure 6 is a chart of volumetric Power in W/'cm3 versus Current density in A/g,
DETAIL D DESCRIPTION OS* THE ΣΜΨΕΒΊΙ Μ
The instant invention deals with the addition of graphene into activated carbon, The carbon useful herein has an average size of between 10. nanometer and 100 microns and a BET surface area greater than about 300 m2/g. The graphene has a size between 30 nanometers and 50 microns and a BET surface of greater than about 300 mVg. In addition/ the graphene has an aspect ratio between about 25 and 25,000. The graphene to carbon ratio is between 0,5 and 10. In Figures I to 6, 1 designates 100% YP50F 2 designates 90% YP50F and 10% C7-5.0; 3 designates 80% YP50F and 20% C?50; 4 designates 70% YP50F and 30% C7S0; 5 designates 60% YP50F and 40% C750; 6 designates 50% YP50F and 50% C75Q, weight ratios.
In Figures 7 and. 8„ I designates 100% xGnP Xg Sciences grapheme; 2 designates '90% activated carbon and 10% xGnP 3 designates 100% Kansai activated carbon; and 4 designates 100% YP50F activated carbon. Example 1
Commercial activated carbon (ACTIVATED CARBON; YP-5QF,
ISGOmVg, urary Chemical Company} and nanosiaad graphene; C~750, 750m2/g, XG Sciences,. Lansing, Michigan) were used as the active materials in this example. Carbon black (Super C, Timcal ) and PVDF were used as conductive agents and polymeric binder, respectively. The paste consisting of typical weight ratio of active carbon: nano sized graphene : Super-Ci PVDF ~ 88:7:5 was coated o aluminum foil via a doctor blade method. Galvanostatic charge/discharge for electrochemical characterization was performed in 1M TE/ABF-s/acetonitriie electrolyte in the range of 0 * 2.5V.
While no synergic effect for the hydbridization of nano sized graphene with activated carbon was shown at low current density {<A/'g} , the capacitance of nano sized graphene/activated carbon electrode was increased over activated carbo alone electrode at high current density (>lA/g) . The addition of 30% to 40% of nano sized graphene seems optimal to achieve the best synergic effect. See Figures 1 and 2. Energy density was compared. The behavior of gravimetric energy density as a function of current density was similar to that of capacitance. However., the volumetric energy density of nano sized .graphene/activated carbon electrode was higher than that of activated carbon electrode regardless of current
density.
Power density was compared. Both gravimetric and volumetric powder density were increased for the nano sized
graphene/activated carbon electrodes regardless of current density and nano sized graphene content due to excellent
conductivity of the nano sized graphene.
See also Figures 3 and ,
Exam le 2.
Two commercial activated carbons were used as active component: YP-50F (ISOQmVg, uraray Chemical Company and MSP-20 (22QQHrVg, ansai Chemical Company. Manosized graphene {C-750, 75QraVg)- , and multi-walled carbon nanotubes <23.0m2 g, Ranwh
Nanotech) were used as another active material and the binder, respectively. Activated carbon or the activated carbon /nano sized graphene was dispersed in isopropyl alcohol using a bath type so icator for 60 minutes and carbon nano tubes was also separately sonicated in Isopropyl alcohol for 1 hour. The dispersed activated carbon and the carbon nano tubes solutions were combined, followed by additional 60 minutes sonication. Then, the activated carbon-carbon nano tubes and activated carbon/nano sized graphene-carbon nanotubes dispersion (ink) was filtered using a membrane filtration system. After drying at 80 *C under vacuum for 2 hoars, the activated carbon-carbon nano tubes and activated carbon/nano sized graphene-carbon nano tube free standing paper were calendared on Mi foam, Electrochemical tests for 2016 coin cell with two identical activated carbon-
S carbon nano tube electrodes was done in IM TEABF^ acetonltrile electrolyte-
The specific capacitance and energy density of activated carbon/narao sized graphene-carbon nano tube electrode shows higher than that of activated carbon-carbon nano tube
electrodes, which confirms the synergistic effect of the hybridisation of activated carbon-nano sized graphene as co- active materials for electrochemical capacitors, See Figures 5 and 6.

Claims

at is claimed is;
I. A composition of matter comprising a combination of a high surface area nanosized .graphite, and carbon wherein the nanosized graphite is selected from the group consisting of nanosized grapheme nanot'uhes and nanosized grapheme
nanopiatelets .
A composit.ion of matter as claimed in claim 1 wherein the carbon is selected from the group consisting essentially of:
a. activated carbon;
b. carbon black, and,
c carbon nanofibers, and,
d. carbon aerogels.
process of manufacturing a composition as claimed in claim 3, said method comprising:
i. dispersing graphene in a suitable solvent;
ii. dispersing carbon in a suitable solvent,
iii. combine and mix the products of i and ii to form a slurry
iv. filtering said slurry to provide a sheet form; v. drying the sheet formed in iv.;
vi. calendaring said sheet to a desired thickness and surface finish.
PCT/US2014/025594 2013-03-15 2014-03-13 Graphene / carbon compositions Ceased WO2014151372A1 (en)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP14769687.6A EP2973805A4 (en) 2013-03-15 2014-03-13 Graphene / carbon compositions
KR1020157029176A KR20150132394A (en) 2013-03-15 2014-03-13 Graphene / carbon compositions
JP2016501889A JP2016518705A (en) 2013-03-15 2014-03-13 Graphene / carbon composition
CN201480022773.8A CN105122520A (en) 2013-03-15 2014-03-13 Graphene/carbon compositions

Applications Claiming Priority (4)

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US201361786735P 2013-03-15 2013-03-15
US61/786,735 2013-03-15
US14/201,986 US20140299818A1 (en) 2013-03-15 2014-03-10 Graphene / carbon compositions
US14/201,986 2014-03-10

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EP2973805A1 (en) 2016-01-20
KR20150132394A (en) 2015-11-25
EP2973805A4 (en) 2016-12-07
TW201446644A (en) 2014-12-16
US20140299818A1 (en) 2014-10-09
JP2016518705A (en) 2016-06-23
CN105122520A (en) 2015-12-02

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