Source: http://www.google.com/patents/US7348096?dq=5527183
Timestamp: 2015-01-28 12:11:49
Document Index: 195723736

Matched Legal Cases: ['Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60', 'Application No. 60']

Patent US7348096 - Polyethylene glycol diacrylate dissolved in a zinc chloride solution as a ... - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inAdvanced Patent SearchPatentsA flat, flexible electrochemical cell is provided. The within invention describes various aspects of the flat, flexible electrochemical cell. A printed anode is provided that obviates the need for a discrete anode current collector, thereby reducing the size of the battery. An advantageous electrolyte...http://www.google.com/patents/US7348096?utm_source=gb-gplus-sharePatent US7348096 - Polyethylene glycol diacrylate dissolved in a zinc chloride solution as a gelled material for carbon zinc batteryAdvanced Patent SearchPublication numberUS7348096 B2Publication typeGrantApplication numberUS 10/321,182Publication dateMar 25, 2008Filing dateDec 17, 2002Priority dateFeb 12, 2002Fee statusPaidAlso published asCA2513454A1, CN1659726A, CN100367539C, EP1485960A2, EP1485960B1, EP2276092A1, EP2276092B1, US7625664, US7727290, US8119278, US20030165744, US20060115717, US20100040941, US20100209756, US20110274959, US20120107666, WO2003069700A2, WO2003069700A3Publication number10321182, 321182, US 7348096 B2, US 7348096B2, US-B2-7348096, US7348096 B2, US7348096B2InventorsMark A. Schubert, Jing Zhang, Guanghong Zheng, Frank H. Feddrix, Richard A. Langan, Frank B. Tudron, Gary R. Tucholski, Abdelkader Hilmi, John C. Bailey, Andrew WebberOriginal AssigneeEveready Battery Company, Inc.Export CitationBiBTeX, EndNote, RefManPatent Citations (23), Referenced by (5), Classifications (74), Legal Events (2) External Links: USPTO, USPTO Assignment, EspacenetPolyethylene glycol diacrylate dissolved in a zinc chloride solution as a gelled material for carbon zinc batteryUS 7348096 B2Abstract A flat, flexible electrochemical cell is provided. The within invention describes various aspects of the flat, flexible electrochemical cell. A printed anode is provided that obviates the need for a discrete anode current collector, thereby reducing the size of the battery. An advantageous electrolyte is provided that enables the use of a metallic cathode current collector, thereby improving the performance of the battery. Printable gelled electrolytes and separators are provided, enabling the construction of both co-facial and co-planar batteries. Cell contacts are provided that reduce the potential for electrolyte creepage in the flat, flexible electrochemical cells of the within invention.
1. A flat flexible battery comprising an electrode, at least one electrode internal current collector having first and second ends and at least one electrode external terminal having first and second ends, and a flexible nonconductive packaging material, said packaging material sealed together at at least one seal junction to form a seal area and a sealed housing surrounding said electrode, wherein said internal current collector and said external terminal are discrete structures, and wherein said internal current collector first end contacts said electrode, said internal current collector second end is positioned within said seal junction, said external terminal first end is positioned within said seal junction and said external terminal second end is positioned external said seal junction and external said housing wherein said internal current collector and said external terminal are not in physical contact within said seal junction.
2. The battery of claim 1, further comprising an electrically conductive medium disposed between the second end of the internal current collector and the first end of the external terminal.
3. The battery as defined in claim 2, wherein the electrically conductive medium comprises electrically conductive adhesive.
4. The battery as defined in claim 2, wherein the electrically conductive medium comprises epoxy. Description
RELATED APPLICATIONS This application claims benefit under 35 USC 119(e) to the following U.S. provisional patent applications: U.S. Pat. Application No. 60/356,407, U.S. Pat. Application No. 60/356,236, U.S. Pat. Application No. 60/356,213, U.S. Pat. Application No. 60/356,406, U.S. Pat. Application No. 60/356,583, U.S. Pat. Application No. 60/356,247, U.S. Pat. Application No. 60/356,266, and U.S. Pat. Application No. 60/356,584, all filed on Feb. 12, 2002 and pending.
FIELD OF THE INVENTION This invention relates to a flexible thin battery and device and a method for making such a battery and device. More specifically, this invention relates to a flexible thin printed battery wherein one or more of the electrodes are printed onto a flexible substrate using a printable ink, and to devices powered by such batteries.
BACKGROUND OF THE INVENTION Flexible planar thin batteries utilizing lithium-based chemistries are known wherein the electrodes are formulated by the deposition of an active material film onto a substrate using various deposition techniques such as pulsed laser deposition, spin coating and sputtering. These techniques tend to require relatively costly and complex equipment and do not lend themselves to a high throughput inexpensive manufacturing process. Further, many devices requiring a power supply, such as novelty packaging and greeting cards augmented with audio and/or visual outputs, are manufactured on high speed web-based printing lines. Lithium-based technologies are not an attractive power source for such low cost per unit applications. The ability to produce both the device and the power supply in a single process presents opportunities for cost savings. There is therefore a need to develop an inexpensive electrochemical power supply that can be produced in a web-based process by stenciling, screen printing or other thick film application processes. As used herein, �print� and �printing� and �printable� refer to any such thick film application process whereby the layer produced is between 10 and 250 microns thick and includes both stenciling and screen printing processes.
SUMMARY OF THE INVENTION A thin, flexible printed battery is provided comprising at least one printed electrode that can be a printed anode or a printed cathode assembly and an electrolyte contained within a sealed housing or package and further comprising external contacts or tabs to provide current from the battery to the battery powered device. The electrode assembly can incorporate either a coplanar or a cofacial electrode arrangement.
DESCRIPTION OF THE DRAWINGS FIG. 1A is an electrochemical cell according to the within invention.
FIG. 1B is a cross sectional view of FIG. 1A as indicated.
FIG. 2 is an electrochemical cell with cell contacts according to an embodiment of the within invention.
FIG. 3 is an electrochemical cell with cell contacts according to an alternate embodiment of the within invention.
FIG. 4 is an electrochemical cell with cell contacts according to another alternate embodiment of the within invention.
FIG. 5 is an electrochemical cell with cell contacts according to another alternate embodiment of the within invention.
FIG. 6A is an electrochemical cell with cell contacts according to another alternate embodiment of the within invention.
FIG. 6B is an electrochemical cell with cell contacts according to another alternate embodiment of the within invention.
FIG. 7 is a printed anode and zinc mesh tab according to the within invention.
FIG. 8 is a printed cathode current collector and tab according to the within invention.
FIG. 9 is a co-planar printed anode and cathode according to the within invention.
FIG. 10 is a circular co-planar anode and cathode according to the within invention.
FIG. 11 is a graph of internal resistance for cells using a gelled electrolyte versus a liquid electrolyte.
FIG. 12 is the printed circuitry for a sound card device powered by a printed cell according to the within invention.
FIG. 13 is the final circuit for a sound card device powered by a printed cell according to the within invention.
FIG. 14 is a graph comparing the thixotropic properties of a polymer electrolyte using polyethylene oxide versus fumed silica as a viscosifying agent.
FIG. 15 is a plot of required cathode area and discharge efficiency as a function of the weight percent of graphite for an aqueous based cathode ink at a given cathode thickness.
DESCRIPTION OF THE PREFERRED EMBODIMENT Components of the thin flexible printed battery 1 of the within invention include a printed anode 3, a printed cathode 5, a cathode current collector 7, a separator 9 and an aqueous electrolyte contained within a flexible thin battery package, housing or enclosure 11. See FIG. 1A and FIG. 1B.
In addition to a binder and solvent system, the zinc ink of the within invention can further include other cell additives to produce beneficial performance attributes. For example, the relatively fine particle size of the zinc employed in the zinc ink of the within invention results in increased gassing. A surfactant known to reduce gassing in alkaline cells has both a phosphate group and polyethylene oxide and/or polypropylene oxide chains. Such a surfactant is available commercially under the Union Carbide tradename Triton QS-44. We have discovered that surfactants of this type are even more beneficial in controlling gassing in acidic electrolytes such as LeClanche or zinc chloride electrolytes. As used herein, a �LeClanche electrolyte� is an electrolyte containing both zinc chloride and ammonium chloride.
100 cycles (1 cycle = 6 sec. at 2 mA and 60
sec. off)
100 cycles (1 cycle = 16 sec. at 8 mA and 60
TABLE II (co-facial electrodes): Minimum required cathode Test current collector thickness 100 cycles (1 cycle = 6 sec. at 2 mA and 60 6-8 microns sec. off) 100 cycles (1 cycle = 16 sec. at 8 mA and 60 24-30 microns sec. off) The resistance of these collectors and their resulting performance are a function of the drying conditions utilized.
Once an appropriate collector is printed onto the substrate, the cathode ink is then printed onto the printed current collector. The cathode ink formulation is a mixture of EMD, binder and conductor in an aqueous or a non-aqueous solvent. The EMD powder utilized will depend on the targeted electrode thickness, desired discharge efficiency and intended application for the cell. Non-milled EMD with a d(50) of around 40 microns is unsuitable for a printed cathode with a targeted thickness of 50 microns or less. EMD with a d(50) measurement of around 1 micron can be obtained by jet-milling the EMD. Such a process is available from, for example, Sturtevant, Inc. in Hanover Mass.
We have further discovered that a low molecular weight polyethylene glycol (PEG) based polymer dissolved in a zinc chloride solution and crosslinked via UV exposure leads to a gelled material that can be printed directly onto a printed electrode in a carbon zinc cell according to the within invention. The preferred polymer is a polyethylene glycol diacrylate as is available from, for example, Sartomer Company, Exton Pa. The PEG diacrylate material of the within invention has the following structure:
10% SR610 PEG diacrylate 6% 600,000MW PEO 0.5% Irgacure 184 0.1% Triton QS 44 83% electrolyte (28% ZnCl2)
In an alkaline system using an alkaline electrolyte such as a standard potassium hydroxide solution, a gelled separator has been discovered. Thus, the present invention provides a primary electrochemical cell comprising at least one printed electrode, where the electrodes are separated by a separator which is electrically insulating but ionically conducting, characterised in that the separator comprises a copolymer of: (1) an ethylenically unsaturated carboxylic acid of formula (I):
EXAMPLE 1 All Percents are by Weight Unless Otherwise Indicated Cells were made according to this example. The anode ink wet formulation was 9.6 percent zinc acetate dihydrate, 31.7 percent water, 1.3 percent PVP (molecular weight of 2.2 to 2.8 million) and 57.4 percent zinc dust. The zinc ink was made by first combining the zinc acetate dihydrate obtained from Aldrich Chemical Company with water to form an aqueous solution. PVP was added to the aqueous solution to make a viscous salt-polymer solution. Zinc dust added and the mixture was stirred until homogeneous. The zinc dust was leaded with 0.16 percent lead. The zinc dust had a Microtrac average volumetric particle size, or d(50) value of about 10 microns. The mixture was allowed to stand to achieve the appropriate thickness, about 90 to 120 minutes. An anode was then screen printed by hand. The anode substrate was the inner heat sealable surface of a flexible polymer and metal laminate packaging material available from Pharma Center Shelbyville, product number 95014. The laminate comprises an inner heat sealable ethylene acrylic acid layer, a layer of aluminum, and an outer protective polymer layer. Four to five wet passes over the screen resulted in an anode 39 millimeters�37 millimeters with a thickness of about 0.087 millimeters. The anode was dried at 70� C. for five minutes. An anode tab 23 made of 0.002 inch thick zinc mesh was adhesively attached to the substrate 25 for place holding until the anode ink 27 was printed onto the substrate, overlapping one end of the tab and thereby affixing it to the substrate. See FIG. 7, illustrating the zinc mesh external tab 23 and the anode ink 27, prior to trimming the part for assembly into a cell. Alternatively, the anode tab 23 could also be printed silver ink.
EXAMPLE 2 Co-planar electrode assembly cells were constructed according to this example. An anode was printed using the same anode ink formulation and substrate as in Example 1, and a 0.002 inch thick zinc mesh anode current collector as in Example 1 was affixed to the substrate in the same manner as in Example 1. The anode 34 was screen printed to a size of 50.4 millimeters�6.8 millimeters with an average thickness of 109 millimeters. The cathode current collector and cathode were stenciled using the same formulation as in Example 1 onto the same substrate as the anode to form a co-planar electrode arrangement. The cathode current collector 35 was stenciled to a size of 40 millimeters�27 millimeters�0.036 millimeters, while the cathode ink 37 was stenciled onto the current collector with a thickness of 0.166 millimeters. See FIG. 9. The gap between the cathode and the anode was 2.0 millimeters. The electrode surfaces were wetted up with the same electrolyte as in Example 1, and the same separator paper as in Example 1 was introduced to provide an electrolyte soakup such that a total of 0.6 to 0.7 grams of electrolyte was introduced into the cell. The separator paper in this co-planar arrangement is sized to cover both the anode and the cathode.
EXAMPLE 3 Co-facial electrode assembly cells were constructed as follows. A zinc mesh anode was utilized in the cells of this example, consisting of a 0.005 inch thick piece of zinc mesh available from Delkar Corporation. The mesh was cut to 39 millimeters�37 millimeters and adhered to the same substrate material as in Examples 1 and 2. The anode current collector was formed from this zinc mesh also and adhered to the substrate in the same manner.
EXAMPLE 4 Zinc Chloride Electrolyte Cells with an Aqueous Zinc Ink Co-Solvent Formulation Cells were constructed utilizing an aqueous zinc ink formulation with a co-solvent system in accordance with the within invention. The cells had a printed zinc anode, a printed manganese dioxide cathode, a zinc chloride electrolyte and a coated kraft paper separator as described above. The electrolyte was a 28 weight percent zinc chloride solution to which 600 ppm lead chloride and 1000 ppm cetyltrimethylammoniium bromide (available from Aldrich) was added. This solution was filtered to remove solids prior to introduction into the cells. A co-solvent system comprising water and NMP was utilized with a PVP binder in the zinc ink formulation. The anode zinc ink general formulation was 8.6 grams Union Miniere zinc dust (1600 ppm lead) with a laser median diameter of 10.2 microns, 0.2 grams PVP K-120, 4.5 mL 1.4 molar zinc acetate aqueous solution and 0.5 mL NMP. The cathode ink general formulation was 7 grams Chemetals jet-milled EMD (d(50)<1 micron, d(90)<3 microns), 2.8 grams synthetic graphite KS6, 0.2 grams PVP K-120 and 10 mL water. The actual zinc and EMD inputs per cell are listed in Table VI. The anode tab silver ink (Acheson Colloids, Electrodag 479SS, except where otherwise noted) and the cathode tab and current collector ink (Acheson Colloids, Electrodag PF407C) were printed onto the sealing surface of a metal laminated packaging material available from Pharma Center Shelbyville, product number 95014, and dried. The cathode ink and the anode ink as described above were printed onto the respective collectors and the cells were assembled into a co-facial arrangement and a separator was placed between the electrodes. The cells were trimmed, heat sealed along three sides, about 0.7 to 0.8 grams of the electrolyte was dispensed into the cell and the cell was sealed. The cells were discharged for 100 cycles and the results are presented in Table VII:
Pass 8 mA pulse test for 100 cycles @ 16 sec. on/60 sec. off.
Pass 15 mA pulse test for 100 cycles @ 16 sec. on/60 sec. off.
EXAMPLE 5 Cells Using a Zinc Acetate Electrolyte Cells were constructed utilizing a zinc acetate electrolyte solution with printed anodes and cathodes. The general formulation for the printed zinc ink anode was 8.6 grams Union Miniere zinc dust (1600 ppm lead) with a laser median diameter of 10.2 microns, 0.2 grams PVP K-120 and 5.0 mL 1.4 molar zinc acetate aqueous solution. The actual zinc input per cell is indicated in Table VIII. The non-aqueous cathode ink formulations are as noted in the table�jet-milled EMD (purchased from Chemetals product K60 and jet-milled by Sturtevant, Inc., in Hanover, Mass.) with an average particle size of between 0.3 and 1.0 microns and non-milled EMD (purchased from Kerr McGee) with an average particle size of about 40 microns are both used in these cells. The anode was printed directly onto the packaging laminate as in Example 1. The cathode collector and the anode and cathode tabs consisted of printed silver ink (Electrodag 479SS from Acheson Colloids). The cells were assembled into a co-facial electrode assembly with a coated kraft paper separator as described in example 8. The cells were partially sealed, the electrolyte was introduced and the cells were completely sealed. The results of a signature discharge test are reported in Table VIII, where a signature discharge test is defined in general as a discharge sequence from high to low rate with a 30 minute rest time in between each discharge.
Cathode eff. 10.57% @ 20 mA/1.43 mA/cm2 Cathode eff. 3.23% @ 10 mA/0.71 mA/cm2 Cathode eff. 3.50% @ 5 mA/0.36 mA/cm2 Cathode eff. 6.56% @ 2 mA/0.14 mA/cm2 Cathode eff. 6.00% @ 1 mA/0.07 mA/cm2 .2573
Cathode eff. 11.21% @ 20 mA/1.43 mA/cm2
Cathode eff. 3.75% @ 10 mA/0.71 mA/cm2
Cathode eff. 3.74% @ 5 mA/0.36 mA/cm2
Cathode eff. 7.64% @ 2 mA/0.14 mA/cm2
Cathode eff. 8.08% @ 1 mA/0.07 mA/cm2
Cathode eff. 27.57% @ 20 mA/1.43 mA/cm2 Cathode eff. 28.40% @ 10 mA/0.71 mA/cm2 Cathode eff. 3.23% @ 5 mA/0.36 mA/cm2 Cathode eff. 3.28% @ 2 mA/0.14 mA/cm2 Cathode eff. 1.75% @ 1 mA/0.07 mA/cm2 .1927
Cathode eff. 56.73% @ 20 mA/1.43 mA/cm2 Cathode eff. 4.85% @ 10 mA/0.71 mA/cm2 Cathode eff. 4.55% @ 5 mA/0.36 mA/cm2 Cathode eff. 5.35% @ 2 mA/0.14 mA/cm2 Cathode eff. 3.48% @ 1 mA/0.07 mA/cm2 AGeneral cathode ink formulation: 9.2 grams Kerr McGee non-milled EMD, 0.6 grams synthetic graphite KS6, 0.2 grams Kureha 1100 PVDF binder, 3.3 mL NMP solvent.
EXAMPLE 6 Co-Planar Cell with Gelled Zinc Chloride Electrolyte A gelled electrolyte was prepared as follows: a 6.0 weight percent Galactasol solution was gradually added to 28% ZnCl2 solution contained in a beaker. The solution was stirred with a magnet bar to mix the electrolyte. Then the gelled electrolyte was left at room temperature overnight to let the trapped air escape. The degassing process could be speeded up by putting the gelled electrolyte in a vacuum oven. Coplanar cells with circular electrodes were constructed as follows: Circular cathodes 39 with a diameter of ⅜ inch (9.525 mm) were printed on a strip 41 of Grafoil manufactured by UCAR, Inc. (ca. 25 mm�100 mm, 0.142 mm) with stencils. The printed cathode thickness varies from 0.002 inches to 0.008 inches. Then the Grafoil strips with dried cathodes were trimmed to fit the cathode size with a narrow tab as the current collector as demonstrated in FIG. 10. A piece of zinc foil with 0.003 inch thickness was cut to a shape as the anode 43. Then the cathode 39 and the anode 43 were placed on a piece of book tape. The gap between the cathode and the anode was about 1 millimeter. The Galactasol gelled electrolyte was placed on the top of the electrodes. Finally, another piece of book tape was placed on the top of the assembly to seal the cells.
EXAMPLE 7 Alkaline Cells with a Polymer Separator and a Zinc Ink Having Excess +2 Zinc Ions Co-facial cells were constructed with and without the addition of excess +2 zinc ions to the anode ink formulation to compare performance. All the cells included a copolymer separator comprising a 20:80 molar ratio of acrylic acid and sodium styrene sulphonate. The gel is formed by combining the copolymers in the above molar ratio with water so that the resulting solution is 20 weight percent copolymer, 80 weight percent water. The anode and the cathode are each initially coated with the copolymer gel to form an adhesive layer approximately 0.001 inch thick. While these layers are still wet, a free-standing co-polymer film of a thickness as indicated in Table IX was placed onto one of the wet layers and the cell was then assembled in a co-facial arrangement, with the wet co-polymer layers additionally providing adhesive properties. The free-standing film was formed by applying a doctor blade to the above gel on glass and coagulating the film by dipping the glass into a 37-40 weight percent potassium hydroxide bath.
TABLE IX (alkaline cells with co-polymer separator and zinc ink having excess +2 zinc ions) Anode input Cathode input (grams zinc) (grams EMD) Polymer separator Test results Lot 4241-1 .8367 .1073 .008 inches IR drop (180 mV) > mass transfer > activation Lot 4241-2 .5856 .1364 .024 inches IR drop (120 mV) > mass transfer > activation Lot 4241-3 .6315 .2036 .008 inches Mass transfer > IR drop (20 mV) > activation Lot 4241-4 .6497 .1840 .024 inches Mass transfer > IR drop (80 mV) > activation The addition of zinc chloride into the zinc ink increases the printed anode conductivity and lowers the ohmic resistance.
EXAMPLE 8 Sound Card Circuit A printed cell is assembled as follows: initially, a cathode collector is printed onto the sealing surface of a single sheet of a metal laminated packaging material available from Pharma Center Shelbyville, product number 95014, and dried. The cathode current collector is Electrodag PF-407C, a carbon polymer ink available from Acheson. The cathode collector is printed to a dry thickness of 36 microns�27 millimeters�40 millimeters. Next, silver external tabs for the anode and cathode are printed onto the sealing surface of the same sheet of metal laminate and dried. The cathode tab overlaps the cathode current collector ink already deposited onto the metal laminate surface. The silver ink is Acheson 479SS, and each tab has a dry dimension of 32.3 millimeters�11.0 millimeters�10.0 microns thick, and is separated from the other by 11 millimeters. An anode is printed on the same laminate sheet. The anode is a zinc ink with a wet composition of 57.35 weight percent Union Miniere zinc dust with a laser median diameter of 10 microns as reported by the manufacturer, 1.33 weight percent PVP, 31.74 weight percent water and 9.58 weight percent zinc acetate available from Aldrich as Zn(OOOCH3)2.2H2O. The ink is made by first mixing the aqueous zinc acetate solution first, then dissolving the PVP into the solution, and finally adding the zinc dust and stirring until homogeneously mixed. The anode is printed onto the substrate material, overlapping the silver anode tab already deposited on the sealing surface of the metal laminate to a dry thickness of 100 microns�6 millimeters�38.6 millimeters. One of skill in the art will recognize that the order of printing can be changed, and the silver external tabs can be printed initially directly onto the sealing surface without departing from the scope of the within invention.
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