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WO2001056101A1 - Electrolytes pour systeme de stockage d'energie a graphite double - Google Patents

Electrolytes pour systeme de stockage d'energie a graphite double Download PDF

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Publication number
WO2001056101A1
WO2001056101A1 PCT/US2001/002533 US0102533W WO0156101A1 WO 2001056101 A1 WO2001056101 A1 WO 2001056101A1 US 0102533 W US0102533 W US 0102533W WO 0156101 A1 WO0156101 A1 WO 0156101A1
Authority
WO
WIPO (PCT)
Prior art keywords
electrolyte
solvent
carbonate
electrolyte according
cyclic
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/US2001/002533
Other languages
English (en)
Inventor
Lisa Marie Massaro
Thongkhahn P. Lewandowski
Sui-Yang Huang
Gregory Kenneth Maclean
Heather N. Ellis
William E. Orabone, Jr.
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LION COMPACT ENERGY Inc
Original Assignee
LION COMPACT ENERGY Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LION COMPACT ENERGY Inc filed Critical LION COMPACT ENERGY Inc
Priority to CA002365631A priority Critical patent/CA2365631A1/fr
Priority to EP01903331A priority patent/EP1183746A1/fr
Priority to AU2001231161A priority patent/AU2001231161A1/en
Priority to JP2001555155A priority patent/JP2003521102A/ja
Publication of WO2001056101A1 publication Critical patent/WO2001056101A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • 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
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention relates to energy storage cells. More specifically, the present invention relates to dual graphite energy storage cells.
  • dual graphite energy storage systems require that an electrolyte be chosen specifically for it's use.
  • the carbonaceous material and electrolyte chosen for dual graphite systems are used strictly to intercalate and deintercalate both cations and anions at two different electrodes.
  • the ions are strictly drawn out of the electrolyte solution for intercalation, and never from one electrode to the other.
  • the cations migrate and intercalate into one electrode at the same time the anions migrate and intercalate into the other electrode.
  • the reverse process also occurs simultaneously. This explains why many skilled in the art refer to this technology as dual intercalating.
  • Dual graphite, or dual intercalating, energy storage systems are not dependent upon an electrochemical reaction. These systems also blur the lines of what are commonly used terms of anode or cathode. Instead, those skilled in the art of dual graphite systems refer to the electrodes as "anion intercalating fiber" and "cation intercalating fiber".
  • dual graphite systems do not fit the well known, and well used, term of "an electrochemical cell", and in fact, while the ability to store energy does fit the definition of a battery, the dual graphite systems to do not adhere to the stricter more detailed definitions of batteries that most in the battery art are familiar with using.
  • solvents to be used in electrolytes for dual graphite cells were mostly chosen for application testing because they were common in the battery industry for other technologies.
  • the electrolytes and carbonaceous materials used in dual graphite systems require a unique selection process that is inherent with the technology, since all cell component requirements are interdependent. Through extensive testing, the inventors have proven that the results of individual half cells do not predict the final result of a full dual graphite cell. All components in the dual graphite technology are interdependent, including the cation intercalating carbon fiber, the anion intercalating carbon fiber, and the electrolyte which is composed of an ionizable salt and its concentration, and the solvent. Therefore, the results of the prior art are not indicative of results in a full dual graphite cell.
  • Energy storage is greatly enhanced by the proper selection of electrolytes.
  • Increasing the electrolyte capabilities means that less volume and weight of the material can be required to achieve more energy storage. This in turn increases the entire device's energy density giving the device more energy per weight and volume.
  • less total solvent material in the device reduces the total cost of device.
  • an electrolyte recirculation system including a salt concentration monitor, a pump, and a salt reservoir. Also provided by the present invention is an electrolyte for use in a dual graphite cell, the electrolyte being made of a solvent that dissolves greater than 15 wt% salt. There is also provided an electrolyte for use in a dual graphite cell, the electrolyte being made of a solvent which is stable above 5 V. Also providing is an electrolyte for use in a
  • the electrolyte including a multiple solvent electrolyte that dissolves in at least 15 wt% LiCIO 4 .
  • Figure 1 is a graph showing electrolyte characteristics by the anion capacity versus conductivity of the electrolytes.
  • the present invention provides an electrolyte recirculation system for maintaining proper electrolyte concentration.
  • the electrolyte recirculation system includes a salt concentration monitor, a pump and a salt reservoir.
  • the dual graphite system requires specific electrolytes for optimal results. While a wide range of options exist, extensive appropriate testing, theoretical design, and other factors help to design an electrolyte that is most appropriate for the dual graphite system. Testing for any, or any number of, properties is always performed using a complete dual graphite cell or battery system with a design of experiment in place. Data analysis is accomplished through extensive statistical analysis and patterns thus seen where possible. The other factors involved are those set by the inventors as reasonable constraints for consumer goods and performance criteria. These include items such as safety, salt dissolution capability, conductivity, voltage stability, and high capacity (anionic and cationic).
  • salts chosen for use in dual graphite electrolytes must be readily ionizable, at least relatively voltage stable, dissolvable in the chosen solvent to a minimum of 15 wt% (depending upon cell design), and intercalatable. Also, the solvents chosen for use in dual graphite electrolytes must support the above needs of the salt, in addition to itself having a voltage stability that is appropriate for the dual graphite system.
  • a pattern has been found in electrolytes with salt concentrations of 25 weight percent and greater. At these high concentrations, single solvents and the interactions with the salts to provide anion intercalation have been shown to be tied very closely to the solvent dipole moment and the electrolyte conductivity. Following a few easily measurable or calculable physical properties there is provided a model that can be run on any candidate solvent to determine if the solvent has the ability to give the desired capacity results without having to spend time, money and materials to test every imaginable solvent in a dual graphite cell.
  • the single solvent electrolyte systems that have been proven to provide dual graphite capacity for anion and cation intercalation must meet the following qualifications.
  • Acyclic solvents with dipole moments of less than 2.0 dynes which are measured or calculated using the DelRe model or CNDO open shell model, that when blended with the salt have a conductivity of greater than 0.5mS/cm.
  • Examples of acyclic solvents include, but are not limited to, dimethyl carbonate, dimethyl sulfite, methyl acetate, and ethyl methyl carbonate.
  • Cyclic solvents with dipole moments between 7.0 and 4.5 dynes are measured or calculated using the DelRe model or CNDO open shell model, that when blended with the salt have a conductivity of greater than 2.0mS/cm.
  • Examples of cyclic solvents include, but are not limited to, sulfolane, glycol sulfite, and propylene carbonate.
  • Benzene based compounds studied to date have no dual graphite capacity, in compounds such as pyridine (PY) and toluene (TL) these cyclic solvents fall out of the required dipole moment requirements (PY's is around 2 dynes and TL is around 1 dyne).
  • Other benzene base compounds, such as nitrobenzene (NB), do not dissolve the required amount of salt.
  • a structure is drawn with some modeling software (such as ChemSW ®) and the dipole moment is calculated or it can be experimentally measured. If the dipole moment does not meet the requirements for the structure type, it is not pursued as a capacity enhancing solvent or capacity additive for dual graphite system electrolytes. If the dipole moment does meet the requirements for the structure type, a small electrolyte sample is prepared and conductivity measured. A dual graphite cell is built for capacity measurement only if the requirements are met.
  • some modeling software such as ChemSW ®
  • Capacity enhancing solvents for dual graphite cells meet these requirements: acyclic compounds have ⁇ 2D dipole, >0.5mS/cm conductivity and are able to solubilize at least 25wt% salt; cyclic solvents have 4.5 to 7D dipole, >2mS/cm conductivity, and do not contain a benzene ring and be able to solubilize at least 25wt% salt.
  • additives can be mixed in small portions with the single solvent compounds described above without detrimentally affecting the capacity performance.
  • Additives including non-flammable additives like TEPO (triethylphosphate), or conductive additives like PN (propionitrile); while none of these additives meet the model requirements for capacity enhancement as single solvents themselves, nor do they achieve reasonable capacity upon testing, when used as additives in 10wt% or less quantities are not detrimental to the capacity measured in the supporting solvent (i.e. SL alone measures at least 160mAh/g capacity and when 10wt% TEPO is added to the SL the capacity is the same). In fact they can occasionally improve capacity achieved in the supporting solvent.
  • TEPO triethylphosphate
  • PN propionitrile
  • binary blends of one acyclic and one cyclic carbonate provide reasonable capacity at all blend ratios.
  • EC:DMC ethylene carbonate:dimethyl carbonate
  • Another binary blend pattern is that of two cyclic carbonates mixed together.
  • 15wt% LiCIO4 achieving at least 160mAh/g anion capacity
  • other blends from 10:90 to 90:10 also achieve over 100mAh/g capacity.
  • Another binary blend pattern involves the use of a binary solvent blend using a sulfone, such as sulfolane (SL), or a cyclic carbonate, such as ethylene carbonate, in combination with an ester, such as methyl acetate (MA). While all ratios of these binary blends give dual graphite capacity, the ratio of two parts sulfone or cyclic carbonate to one part ester by weight is the most desirable.
  • a sulfone such as sulfolane (SL)
  • a cyclic carbonate such as ethylene carbonate
  • ester such as methyl acetate
  • sulfone and carbonate blends i.e. SL:PC at 25:75 to 75:25, or
  • ethers such as diethyl or 2-methoxyethyl
  • esters including cyclic esters (for example GBL) cyclic carbonates or acyclic carbonates
  • nitriles for example, propionitrile or 3- methoxypropionitrile
  • sulfones for example, sulfolane, ethyl methyl sulfone, 3-methyl sulfolane, ethyl isopropyl sulfone, etc.
  • sulfoxides such DMSO
  • sulfites such as dimethyl sulfite
  • ketones such as MEK
  • furans for example, THF or dioxane
  • Organophosphates such as TEPO.
  • the most preferred solvents are EC, PC, DMC, DEC, GBL, SL, EMS, MSL, EMC, MA, TEPO, and GS.
  • the least preferred solvents are MEK, MIPK, MF, EA, DMS, DG, DEE, MTHF, and BST.
  • EC:DMC:TEPO especially 67:28:5
  • EC:DMC:GLN especially 67:28:5
  • Electrolytes with high anodic voltages have always been of interest in electrochemical batteries. Dual graphite systems also require high voltage stability. Higher anodic voltage stability provides the dual graphite systems with less solvent degradation which increases cycle life of a cell, and allows for higher possible charge voltages increasing various cell performances such as energy density by increasing the midpoint voltage on discharge. Testing of voltage stability in an electrolyte for use in a dual graphite cell must occur in a dual graphite cell. These test cells then have a graphite working electrode and a graphite counter electrode, while the reference electrode used is lithium metal.
  • the following single solvents with at least 25wt% salt are representative of appropriate voltage stability materials: PC (5V), EC (>5.5V), DMC (4.9V), SL(>5.5V), GS(4.6V), DEE (5.3V), GBL(5.5V).
  • the solvents listed are representative of compounds of that class; for instance DEC & DMC are both acyclic carbonates and both are stable to 4.9V.
  • additives of 10 wt% or less can be used with single solvents without detrimental affects on stability. Additional patterns in dual graphite voltage stability data are seen in binary solvent blends. For example, binary blends of one acyclic and one
  • cyclic carbonate provide similar voltage stability results at all blend ratios.
  • One example is EC: DMC (ethylene carbonate:dimethyl carbonate) with blends from 10:90 to 90:10 by weight with 15wt% LiCIO4 achieving approximately 4.9V, the preferred ratio being 90:10 with a stability of 5.3V.
  • Another binary blend pattern is that of a mixture of 2 cyclic carbonates.
  • One example is EC:PC 33:67 by weight with 15wt% LiCIO4 achieving at least 5.5V stability; other blends from 10:90 to 90:10 also achieve stability over 5V.
  • Another binary blend pattern example involves the use of a binary solvent blend using a sulfone, such as sulfolane (SL), or a cyclic carbonate, such as ethylene carbonate, in combination with an ester, such as methyl acetate (MA). While all ratios of these binary blends give voltage stability greater than 5V, the ratio of 2 parts sulfone or cyclic carbonate to 1 part ester by weight is the most desirable.
  • a sulfone such as sulfolane (SL)
  • a cyclic carbonate such as ethylene carbonate
  • ester such as methyl acetate
  • sulfone and carbonate blends i.e. SLPC at 25:75 to 75:25, or SLDMC at 35:65, or Ethyl Methyl
  • Sulfone:DMC at 50:50 sulfone and nitrile blends (i.e. SL:PN at 90:10), cyclic ester and carbonate blends (i.e. gamma-butyrolactone:DMC at 50:50), EC/PC/TEPO (19:76:5), EC/PC/MA (9:76:15), PC/TEPO (50:50),SL/EC/DMC (6:70:24), and EMC/PC/MA (9:67:24).
  • the most preferred salts for use in dual graphite systems are, in order of preference, LiCIO4, LiPF6, LiBF4, UCF3SO3, or mixtures thereof.
  • Least preferred salts are UCF3CO2, LiAsF6, LiCI, LiBr, Lil, LiSCN.
  • the preferred salt concentration in dual graphite cells is between 15wt% and saturation.
  • the most preferred salt concentration range is from 15 to 40wt% of the electrolyte.
  • Another concern with regard to the energy storage cell is the total weight of the cell. It is therefore necessary to determine methods and mechanisms for limiting the weight of the cell.
  • One method of maintaining electrolyte concentrations during charge and discharge, and to improve cell energy density is to remove the excess solvent from a dual graphite cell. This can be accomplished with an electrolyte recirculation system.
  • all inactive materials have to be eliminated or reduced to minimize cell weight.
  • these materials include the current collector materials, separator, solvent, and packaging.
  • the only active materials that contribute directly to cell capacity are the carbonaceous fibers and the salt.
  • the largest inactive weight contributor is the solvent in the electrolyte solution, which is required to carry the salt. Without a material to aid in ion transfer (such as an organic solvent, ionic liquid, gel, or polymer) the system does not work, since this is the mechanism for intercalation into the graphite materials. Reducing the solvent
  • the salt can come out of solution or its concentration can be too high and thereby reducing the electrolyte conductivity. The more conductive the electrolyte, the more mobile the ions are.
  • an electrolyte recirculation system can be used. This is a system that allows a cell to be continually cycled at the most conductive salt concentration.
  • the recirculation system is designed to replenish and to remove the salt as needed to maintain maximum cell conductivity, which in turn minimizes cell resistance.
  • This system requires a concentration monitor which monitors the salt concentration and allows salt to be removed or added to the electrolyte as needed using a pump.
  • the system also requires that a salt reservoir be maintained which stores any unused salt.
  • the circulation system adds salt at that time.
  • the circulation system removes the excess salt from the cell and stores it in the salt reservoir. This method reduces the required solvent weight, while maintaining optimal dual graphite cell conditions.
  • One circulation system can be tied to one or multiple dual graphite cells or batteries.
  • the electrolyte recirculating system optimizes the cell capacity and the energy density of a dual graphite energy storage system, because the recirculation creates the most conductive salt concentrations without ever depleting the salt supply or ions in the energy storage device.
  • the system replenishes and removes salt as needed to maximize cell conductivity which in turn minimizes cell resistance.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)
  • Inorganic Fibers (AREA)
  • Woven Fabrics (AREA)
  • Arc Welding In General (AREA)
  • Inert Electrodes (AREA)

Abstract

L'invention concerne un système de recirculation d'électrolyte comprenant un appareil de mesure de concentration de sel, une pompe, et un réservoir de sel. L'invention concerne également un électrolyte s'utilisant dans une cellule graphite double, cet électrolyte étant fabriqué à partir d'un solvant qui dissout au moins 15 % en poids du sel est stable au-dessus de 5V et comprend un électrolyte de solvant multiple se dissolvant dans au moins 15 % en poids de LiCLO4.
PCT/US2001/002533 2000-01-26 2001-01-26 Electrolytes pour systeme de stockage d'energie a graphite double Ceased WO2001056101A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
CA002365631A CA2365631A1 (fr) 2000-01-26 2001-01-26 Electrolytes pour systeme de stockage d'energie a graphite double
EP01903331A EP1183746A1 (fr) 2000-01-26 2001-01-26 Electrolytes pour systeme de stockage d'energie a graphite double
AU2001231161A AU2001231161A1 (en) 2000-01-26 2001-01-26 Electrolytes for dual graphite energy storage system
JP2001555155A JP2003521102A (ja) 2000-01-26 2001-01-26 二重グラファイトエネルギー貯蔵型システムのための電解液

Applications Claiming Priority (6)

Application Number Priority Date Filing Date Title
US17824100P 2000-01-26 2000-01-26
US17821700P 2000-01-26 2000-01-26
US17817700P 2000-01-26 2000-01-26
US60/178,177 2000-01-26
US60/178,217 2000-01-26
US60/178,241 2000-01-26

Publications (1)

Publication Number Publication Date
WO2001056101A1 true WO2001056101A1 (fr) 2001-08-02

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Application Number Title Priority Date Filing Date
PCT/US2001/002533 Ceased WO2001056101A1 (fr) 2000-01-26 2001-01-26 Electrolytes pour systeme de stockage d'energie a graphite double
PCT/US2001/002778 Ceased WO2001056100A1 (fr) 2000-01-26 2001-01-26 Fibres de carbone pour batteries au graphite doubles
PCT/US2001/002634 Ceased WO2001054856A1 (fr) 2000-01-26 2001-01-26 Liaison thermique et electrique de faible resistance et son procede de fabrication

Family Applications After (2)

Application Number Title Priority Date Filing Date
PCT/US2001/002778 Ceased WO2001056100A1 (fr) 2000-01-26 2001-01-26 Fibres de carbone pour batteries au graphite doubles
PCT/US2001/002634 Ceased WO2001054856A1 (fr) 2000-01-26 2001-01-26 Liaison thermique et electrique de faible resistance et son procede de fabrication

Country Status (5)

Country Link
EP (3) EP1180067A4 (fr)
JP (3) JP2003520687A (fr)
AU (3) AU2001231185A1 (fr)
CA (3) CA2365630A1 (fr)
WO (3) WO2001056101A1 (fr)

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WO2014104392A1 (fr) * 2012-12-28 2014-07-03 Ricoh Company, Ltd. Élément de stockage électrolytique non aqueux

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US20090233175A1 (en) * 2005-03-31 2009-09-17 Kelley Kurtis C Current Carrier for an Energy Storage Device
GB2469449B (en) * 2009-04-14 2014-06-04 Energy Control Ltd Connecting structure for exteriorly connecting battery cells
DE102011054122A1 (de) * 2011-09-30 2013-04-04 Westfälische Wilhelms Universität Münster Elektrochemische Zelle
US9636986B2 (en) 2012-10-03 2017-05-02 Dana Limited Hybrid drivetrain and method of operation thereof
US9509017B2 (en) * 2014-07-22 2016-11-29 John E. Stauffer Lithium storage battery
WO2017192866A1 (fr) 2016-05-04 2017-11-09 Somnio Global Holdings, Llc Procédés de fabrication additive et dispositifs permettant la fabrication d'objets dotés de renforts de préforme

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Publication number Priority date Publication date Assignee Title
WO2014104392A1 (fr) * 2012-12-28 2014-07-03 Ricoh Company, Ltd. Élément de stockage électrolytique non aqueux

Also Published As

Publication number Publication date
CA2365630A1 (fr) 2001-08-02
WO2001056100A1 (fr) 2001-08-02
CA2368680A1 (fr) 2001-08-02
EP1180067A4 (fr) 2004-03-31
AU2001236560A1 (en) 2001-08-07
EP1180067A1 (fr) 2002-02-20
JP2003521101A (ja) 2003-07-08
AU2001231185A1 (en) 2001-08-07
EP1171923A1 (fr) 2002-01-16
JP2003521102A (ja) 2003-07-08
EP1183746A1 (fr) 2002-03-06
WO2001054856A1 (fr) 2001-08-02
CA2365631A1 (fr) 2001-08-02
JP2003520687A (ja) 2003-07-08
AU2001231161A1 (en) 2001-08-07

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