USH452H - Cathode including a non fluorinated linear chain polymer as the binder, method of making the cathode, and lithium electrochemical cell containing the cathode - Google Patents

Cathode including a non fluorinated linear chain polymer as the binder, method of making the cathode, and lithium electrochemical cell containing the cathode Download PDF

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Publication number
USH452H
USH452H US06/895,015 US89501586A USH452H US H452 H USH452 H US H452H US 89501586 A US89501586 A US 89501586A US H452 H USH452 H US H452H
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Prior art keywords
cathode
linear chain
carbon
solution
electrochemical cell
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US06/895,015
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Edward J. Plichta
Mark Salomon
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US Department of Army
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US Department of Army
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • 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
    • 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
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
    • 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
    • H01M4/043—Processes of manufacture in general involving compressing or compaction
    • 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
    • H01M4/043—Processes of manufacture in general involving compressing or compaction
    • H01M4/0435—Rolling or calendering
    • 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
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • H01M4/621—Binders
    • 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

Definitions

  • This invention relates to a cathode including a non fluorinated linear chain polymer as the binder, to a method of making the cathode, and to a lithium electrochemical cell containing the cathode.
  • Teflon As the binding material. Teflon or polytetrafluoroethylene is expensive although inert, and its use results in cathode structures of poor mechanical stability. These problems do not easily lend themselves to the large scale production of cathodes in manufacturing.
  • the general object of the invention is to provide a cathode suitable for use in lithium electrochemical cells. Another object of the invention is to provide such a cathode that will be mechanically stable and relatively inexpensive to manufacture. A further object of the invention is to provide such a cathode that will be suitable for use in a primary or secondary lithium cell.
  • a cathode for use in lithium primary or secondary cells can be prepared from a mixture of active cathode material, conductive dilutant such as carbon and non fluorinated linear chain polymer.
  • the amount of carbon can be varied depending upon the resistivity of the cathode material and desired porosity of the final cathode structure.
  • Typical cathode materials that can be used are metal halides, oxides and sulfides.
  • the polymer is first dissolved in a non polar solvent such as Decalin (Decahydronaphthalene) or tetrachloroethylene at a temperature near the melting point of the polymer (100° to 150° C.).
  • the active cathode material and carbon are added and the solvent evaporated.
  • the following is a preparation of a cathode structure utilizing TiS 2 as the active cathode material.
  • the procedure is performed in an argon filled dry box.
  • Polypropylene powder is dissolved near its crystalline melting temperature of about 100° to 120° C. in a small volume of decahydronaphthalene of about 5 mils decahydronaphthalene for about 0.1 to 0.2 gm (PP), the solution being stirred continuously during heating. Once the (PP) is dissolved, the solution is removed from the heat and cooled below 100° C. and the active cathode material and carbon powders are then added quickly before the polymer solution cools completely.
  • the powdered materials and solutions are stirred vigorously by hand until the solution is absorbed and the mix becomes granular and has cooled to room temperature.
  • the mixture is then dried in a vacuum oven at about 120° to 150° C. for 12 hours in order to remove the decahydronaphthalene.
  • the dried mixture is then ground into a fine powder and made into cathodes by pressing the powdered mixture onto both sides of an expanded metal screen and then cut to desired dimensions.
  • the TABLE shows typical results for a Li-TiS 2 cell in which cell performance is studied as a function of solvent composition, cathode composition, and cathode preparation, that is, cold-pressing or hot-pressing. Performance is found to be equal to that obtained from cells utilizing cathodes of poor mechanical properties, that is, based on teflon binders.
  • the TABLE shows that one can operate with a wide range of (PP) content in the electrode. More specifically, one can use less binder and still obtain a good mechanically stable cathode. In fact, one can go down to as little as 1 to 3 weight percent of binder which allows one to put in more active cathode material and improve the performance of the cell.
  • the drawing illustrates a cycling profile for a rechargeable lithium cell using a TiS 2 cathode and an electrolyte consisting of 0.8 mol dm -3 LiAlCl 4 in a mixed organic solvent of 24 mass percent 4-butyrolactone in 1,2 dimethoxyethane (24% 4-BL in DME).
  • the cathode 80 mass % TiS 2 , 10 mass % carbon and 10 mass % (PP) is prepared as described in the description of the preferred embodiment.
  • the cell used for the drawing is cycled at 25° C. at a current density of 2.0 mA cm -2 , and excursions are shown for discharges at 5.0 mAcm -2 and at 2.0 mAcm -2 at lower temperatures of -20° C. and -30° C. Cycling is stopped after 33 cycles.
  • the drawing also shows that after excursions to higher current densities and/or lower temperatures, cell performance recovers exceptionally well.
  • the ordinate, percent cathode utilization is an indicator as to how the cell is performing.
  • Any non fluorinated linear chain polymer can be used in the cathode that is stable in the electrolyte of the lithium cell.
  • the linear chain polymers are inert in a wide variety of non aqueous solvents including ethers and lactones. Suitable polymers include (PP) and (PE).
  • Active cathode materials that can be used include metal halides, metal oxides, and metal sulfides of which TiS 2 is preferred. Pure carbon can be used for those cells in which the solvent serves as the depolarizer.
  • any carbon black can be used as the carbon for the cathode that enhances the conductivity of the electrodes.
  • the particular carbon black used in the description of the preferred embodiment is Shawinigan Black but other high surface area carbons or graphite can also be used.
  • the invention even contemplates a cathode made from a mixture of polymer and active cathode material with no carbon present.
  • the electrolyte used in the lithium cell must be compatible with the cathodes made according to the invention.
  • Suitable electrolytes include a solution of an inorganic lithium salt in a pure or mixed organic solvent.
  • mechanically stable structures can be easily prepared by cold-pressing or cold rolling, and by hot-pressing or hot-rolling. Moreover, sintering temperatures below 170° C. should be used since some cathode materials are subject to decomposition above 200° C.
  • non fluorinated linear chain polymers such as (PP) or (PE) can be used to prepare mechanically stable cathodes for nonaqueous lithium cells.
  • the use of the non fluorinated linear chain polymers as binders results in low cost cathodes giving equal electrochemical performance as do Teflon bonded cathodes, but the use of the non fluorinated linear chain polymers results in cathodes having great mechanical stability that can be fabricated in several forms such as plates or rolls, and that can be made as thin as 0.5 mm or less.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

A cathode suitable for use in a lithium electrochemical cell is made from aixture of active cathode material, carbon, and non fluorinated linear chain polymer by a method including the steps of
(A) dissolving the non fluorinated linear chain polymer in a non polar solvent at a temperature near the melting point of the polymer,
(B) adding the active cathode material and carbon and evaporating the solvent, and
(C) grinding the dried mixture into a fine powder and making it into a cathode by pressing the powdered mixture onto both sides of an expanded metal screen and then cutting to the desired dimensions.
The cathode can be combined with lithium as the anode and a solution of 0.8 mol dm-3 LiAlCl4 in a mixed organic solvent of 24 mass percent 4-butyrolactone in 1, 2 dimethoxyethane as the electrolyte to provide a mechanically stable, relatively inexpensive lithium electrochemical cell having good cell performance.

Description

The invention described herein may be manufactured, used, and licensed by or for the Government for governmental purposes without the payment to us of any royalty thereon.
This application is a division of application Ser. No. 749,597, filed June 27, 1985.
This invention relates to a cathode including a non fluorinated linear chain polymer as the binder, to a method of making the cathode, and to a lithium electrochemical cell containing the cathode.
BACKGROUND OF THE INVENTION
Existing technology for the fabrication of cathodes for use in lithium primary and secondary cells utilizes Teflon as the binding material. Teflon or polytetrafluoroethylene is expensive although inert, and its use results in cathode structures of poor mechanical stability. These problems do not easily lend themselves to the large scale production of cathodes in manufacturing.
SUMMARY OF THE INVENTION
The general object of the invention is to provide a cathode suitable for use in lithium electrochemical cells. Another object of the invention is to provide such a cathode that will be mechanically stable and relatively inexpensive to manufacture. A further object of the invention is to provide such a cathode that will be suitable for use in a primary or secondary lithium cell.
It has now been found that the aforementioned objects can be attained by replacing the Teflon binder with a ncn fluorinated linear chain polymer such as polypropylene (PP) or polyethylene (PE).
More particularly, according to the invention, a cathode for use in lithium primary or secondary cells can be prepared from a mixture of active cathode material, conductive dilutant such as carbon and non fluorinated linear chain polymer. The amount of carbon can be varied depending upon the resistivity of the cathode material and desired porosity of the final cathode structure. Typical cathode materials that can be used are metal halides, oxides and sulfides. The polymer is first dissolved in a non polar solvent such as Decalin (Decahydronaphthalene) or tetrachloroethylene at a temperature near the melting point of the polymer (100° to 150° C.). The active cathode material and carbon are added and the solvent evaporated.
DESCRIPTION OF THE PREFERRED EMBODIMENT
The following is a preparation of a cathode structure utilizing TiS2 as the active cathode material. The procedure is performed in an argon filled dry box. Polypropylene powder is dissolved near its crystalline melting temperature of about 100° to 120° C. in a small volume of decahydronaphthalene of about 5 mils decahydronaphthalene for about 0.1 to 0.2 gm (PP), the solution being stirred continuously during heating. Once the (PP) is dissolved, the solution is removed from the heat and cooled below 100° C. and the active cathode material and carbon powders are then added quickly before the polymer solution cools completely. The powdered materials and solutions are stirred vigorously by hand until the solution is absorbed and the mix becomes granular and has cooled to room temperature. The mixture is then dried in a vacuum oven at about 120° to 150° C. for 12 hours in order to remove the decahydronaphthalene. The dried mixture is then ground into a fine powder and made into cathodes by pressing the powdered mixture onto both sides of an expanded metal screen and then cut to desired dimensions.
Although flat plate type electrodes have been prepared in the foregoing embodiment to demonstrate the use of the non fluorinated linear chain polymers as binding materials, the method results in moderately flexible structures which makes the method equally adaptable to the preparation of rolled electrodes, either cold-rolled or rolled through heated rollers using a powdered mix or a slurry mixture using a non reactive organic solvent.
The TABLE shows typical results for a Li-TiS2 cell in which cell performance is studied as a function of solvent composition, cathode composition, and cathode preparation, that is, cold-pressing or hot-pressing. Performance is found to be equal to that obtained from cells utilizing cathodes of poor mechanical properties, that is, based on teflon binders. The TABLE shows that one can operate with a wide range of (PP) content in the electrode. More specifically, one can use less binder and still obtain a good mechanically stable cathode. In fact, one can go down to as little as 1 to 3 weight percent of binder which allows one to put in more active cathode material and improve the performance of the cell.
                                  TABLE                                   
__________________________________________________________________________
Performance Data for Li--TiS.sub.2 Cells Utilizing                        
Polypropylene (PP) as the Cathode Binder.sup.a.                           
Electrode           Mass %                                                
                         Mass %                                           
                              Mass %                                      
                                   Current  Cathode                       
Type.sup.b                                                                
       t/oc                                                               
           Electrolyte                                                    
                    TiS.sub.2                                             
                         Carbon                                           
                              PP   Density: mA/cm.sup.2                   
                                            Efficiency                    
__________________________________________________________________________
cold-pressed                                                              
       25  0.8 mol dm.sup.-3                                              
                    80   10   10   5.0      49.3                          
       25  LiAlCl.sub.4            2.0      75.2                          
       -20 in                      2 0      39.5                          
       -30 24% 4-BL/DME            2.0       5.6                          
cold-pressed                                                              
       25  1.6 mol dm.sup.-3                                              
                    78.5 10   11.5 2.0      66.7                          
       25  LiAsF.sub.6 in          1.0      82.0                          
           2Me--THF                                                       
cold-pressed                                                              
       25  1.3 mol dm.sup.-3                                              
                    83.3 9.6  7.1  1.0      71.1                          
           LiAsF.sub.6 in                                                 
           2Me--THF                                                       
cold-pressed                                                              
       25  1.6 mol dm.sup.-3                                              
                    81.8 12.7 5.5  2.0      69.5                          
           LiAsF.sub.6 in                                                 
           2Me--THF                                                       
cold-pressed                                                              
       25  1.2 mol dm.sup.-3                                              
                    87.3 10.0 2.7  1.0      80.2                          
           LiAsF.sub.6 in                                                 
           2Me--THF                                                       
cold-pressed                                                              
       25  0.85 mol dm.sup.-3                                             
                    79.7 10.1 10.2 2.0      68.9                          
           LiAlCl.sub.4 in                                                
           24% 4-BL/DME                                                   
__________________________________________________________________________
 .sup.a 2Me--THF is 2methyl tetrahydrofuran                               
 DME is 1,2dimethoxyethane                                                
 4BL is 4butyrolactone                                                    
 .sup.b Cathode porosity in the range of 40-60%
DESCRIPTION OF THE DRAWING
The drawing illustrates a cycling profile for a rechargeable lithium cell using a TiS2 cathode and an electrolyte consisting of 0.8 mol dm-3 LiAlCl4 in a mixed organic solvent of 24 mass percent 4-butyrolactone in 1,2 dimethoxyethane (24% 4-BL in DME). The cathode (80 mass % TiS2, 10 mass % carbon and 10 mass % (PP) is prepared as described in the description of the preferred embodiment.
Referring to the drawing, the cell used for the drawing is cycled at 25° C. at a current density of 2.0 mA cm-2, and excursions are shown for discharges at 5.0 mAcm-2 and at 2.0 mAcm-2 at lower temperatures of -20° C. and -30° C. Cycling is stopped after 33 cycles. The drawing also shows that after excursions to higher current densities and/or lower temperatures, cell performance recovers exceptionally well. In the drawing, the ordinate, percent cathode utilization, is an indicator as to how the cell is performing.
Any non fluorinated linear chain polymer can be used in the cathode that is stable in the electrolyte of the lithium cell. The linear chain polymers are inert in a wide variety of non aqueous solvents including ethers and lactones. Suitable polymers include (PP) and (PE).
Active cathode materials that can be used include metal halides, metal oxides, and metal sulfides of which TiS2 is preferred. Pure carbon can be used for those cells in which the solvent serves as the depolarizer.
Any carbon black can be used as the carbon for the cathode that enhances the conductivity of the electrodes. The particular carbon black used in the description of the preferred embodiment is Shawinigan Black but other high surface area carbons or graphite can also be used. The invention even contemplates a cathode made from a mixture of polymer and active cathode material with no carbon present.
The electrolyte used in the lithium cell must be compatible with the cathodes made according to the invention. Suitable electrolytes include a solution of an inorganic lithium salt in a pure or mixed organic solvent.
In the method of the invention, mechanically stable structures can be easily prepared by cold-pressing or cold rolling, and by hot-pressing or hot-rolling. Moreover, sintering temperatures below 170° C. should be used since some cathode materials are subject to decomposition above 200° C.
Thus, it has been demonstrated that non fluorinated linear chain polymers such as (PP) or (PE) can be used to prepare mechanically stable cathodes for nonaqueous lithium cells. The use of the non fluorinated linear chain polymers as binders results in low cost cathodes giving equal electrochemical performance as do Teflon bonded cathodes, but the use of the non fluorinated linear chain polymers results in cathodes having great mechanical stability that can be fabricated in several forms such as plates or rolls, and that can be made as thin as 0.5 mm or less.
We wish it to be understood that we do not desire to be limited to the exact details as described for obvious modifications will occur to a person skilled in the art.

Claims (1)

What is claimed is:
1. Method of preparing a cathode for use in a lithium electrochemical cell from a mixture of TiS2, carbon and polypropylene, said method including the steps of
(A) dissolving polypropylene at 100° to 130° C. in a small volume of decahydronaphthalene contained in an argon filled dry box while stirring the solution continuously during heating,
(B) removing the solution from the heat, cooling to below 100° C., and quickly adding the carbon and TiS2 before the polymer solution cools completely,
(C) stirring the powdered materials and solution vigorously until the solution is absorbed and the mix becomes granular and has cooled to room temperature,
(D) drying the mixture in a vacuum oven at 120° C. to 150° C. for 12 hours in order to remove the decahydronaphthalene, and
(E) grinding the dried mixture into a fine powder and making into a cathode by pressing the powdered mixture onto both sides of an expanded metal screen.
US06/895,015 1985-06-27 1986-08-07 Cathode including a non fluorinated linear chain polymer as the binder, method of making the cathode, and lithium electrochemical cell containing the cathode Abandoned USH452H (en)

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US06/749,597 USH519H (en) 1985-06-27 1985-06-27 Cathode including a non fluorinated linear chain polymer as the binder, method of making the cathode, and lithium electrochemical cell containing the cathode
US06/895,015 USH452H (en) 1985-06-27 1986-08-07 Cathode including a non fluorinated linear chain polymer as the binder, method of making the cathode, and lithium electrochemical cell containing the cathode

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050001357A1 (en) * 1999-10-14 2005-01-06 Nec Tokin Corporation Molded electrode, method for production thereof, and secondary battery using thereof

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3873369A (en) 1973-05-14 1975-03-25 Du Pont Tungsten oxide-containing cathode for non-aqueous galvanic cell
US4201839A (en) 1978-11-01 1980-05-06 Exxon Research And Engineering Co. Cell containing an alkali metal anode, a solid cathode, and a closoborane and/or closocarborane electrolyte
US4223080A (en) 1979-05-11 1980-09-16 Bell Telephone Laboratories, Incorporated Cell and fuel cell electrodes having poly(phosphazene) binder
US4322317A (en) 1980-03-03 1982-03-30 Exxon Research & Engineering Co. Composition for chalcogenide electrodes
US4463072A (en) 1983-11-30 1984-07-31 Allied Corporation Secondary batteries containing room-temperature molten 1,2,3-trialkylimidazolium halide non-aqueous electrolyte
US4499160A (en) 1980-06-05 1985-02-12 Matzliach Babai Cathode and electrochemical cell containing same

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3873369A (en) 1973-05-14 1975-03-25 Du Pont Tungsten oxide-containing cathode for non-aqueous galvanic cell
US4201839A (en) 1978-11-01 1980-05-06 Exxon Research And Engineering Co. Cell containing an alkali metal anode, a solid cathode, and a closoborane and/or closocarborane electrolyte
US4223080A (en) 1979-05-11 1980-09-16 Bell Telephone Laboratories, Incorporated Cell and fuel cell electrodes having poly(phosphazene) binder
US4322317A (en) 1980-03-03 1982-03-30 Exxon Research & Engineering Co. Composition for chalcogenide electrodes
US4499160A (en) 1980-06-05 1985-02-12 Matzliach Babai Cathode and electrochemical cell containing same
US4463072A (en) 1983-11-30 1984-07-31 Allied Corporation Secondary batteries containing room-temperature molten 1,2,3-trialkylimidazolium halide non-aqueous electrolyte

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050001357A1 (en) * 1999-10-14 2005-01-06 Nec Tokin Corporation Molded electrode, method for production thereof, and secondary battery using thereof

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