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`Case 5:20-cv-09341-EJD Document 147-3 Filed 04/08/22 Page 1 of 9
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`EXHIBIT 38
`EXHIBIT 38
`
`

`

`(12) United States Patent
`Krasnov et al.
`
`USOO663.2563B1
`(10) Patent No.:
`US 6,632,563 B1
`(45) Date of Patent:
`Oct. 14, 2003
`
`(54) THIN FILM BATTERY AND METHOD OF
`MANUFACTURE
`(75) Inventors: Victor Krasnov, Tarzana, CA (US);
`y
`Kai-Wei Nieh, Monrovia, CA (US);
`Su-Jen Ting, Encino, CA (US)
`(73) Assignee: Front Edge Technology, Inc., Baldwin
`Park, CA (US)
`Subject to any disclaimer, the term of this
`patent is extended or adjusted under 35
`U.S.C. 154(b) by 11 days.
`
`(*) Notice:
`
`(21) Appl. No.: 09/656,012
`
`Sep. 7, 2000
`(22) Filed:
`(51) Int. Cl." ................................................. H01M 646
`52) U.S. Cl. ................
`... 429/162: 429/127
`S Field of Search
`f 2251 62 ? 27
`
`FR
`E.
`WO
`WO
`
`FOREIGN PATENT DOCUMENTS
`2403652 A 4/1979
`25 G. A g1984
`f2001
`WOOO 60689 A 10/2000
`WO O2 21627 A
`3/2002
`OTHER PUBLICATIONS
`Bolster M-E, et al. “Investigation of lithium intercalation
`metal oxides for thermal batteries' Proceedings of the
`International Power Sources Symposium, Cherry Hill, Jun.
`25–28, 1990; Jun. 25, 1990, pp. 136–140, vol. SYMP. 34,
`IEEE, New York, US.
`Wagner AV, et al. “Fabrication and testing of thermoelectric
`thin film devices' Fifteenth International Conference on
`Thermoelectrics, Pasadena, CA, USA Mar. 26-29, 1996; pp.
`269-273, IEEE, New York, US.
`U.S. Provisional Patent Application entitled, "Comprehen
`sive Patent for the Fabrication of a High Volume, Low Cost
`Energy Products Such as Solid State Lithium Ion Recharge
`
`- - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - - -
`
`s
`
`able Batter, Supercapacitators and Fuel Cells'; filed Mar. 24,
`
`(56)
`
`References Cited
`
`U.S. PATENT DOCUMENTS
`
`3,530,007 A * 9/1970 Golubovic .................. 136/263
`4,543,441. A * 9/1985 Kumada et al. ..
`... 136/244
`5,019,467 A * 5/1991 Fujiwara .................... 29/623.5
`5,338,625 A 8/1994 Bates et al.
`5,445,906 A * 8/1995 Hobson et al. ............ 29/623.3
`5,512,147 A 4/1996 Bates et al.
`5,597.660 A
`1/1997 Bates et al.
`5,612,152 A 3/1997 Bates
`5,705,293 A * 1/1998 Hobson ...................... 429/162
`5,705297 A * 1/1998 Warren ...................... 29/623.4
`6,168,884 B1
`1/2001 Neudecker et al.
`6,280.875 B1 * 8/2001 Kwak et al. ................ 429/124
`
`2000; Ser. No. 60/191,774, Inventors: Jenson, et al.
`(List continued on next page.)
`Primary Examiner Patrick Ryan
`ASSistant Examiner-Gregg Cantelmo
`(74) Attorney, Agent, or Firm Ashok K. Janah
`(57)
`ABSTRACT
`A thin film battery 10 comprises a Substrate 12 which
`permits the battery 10 to be fabricated to provide higher
`energy density. In one embodiment, the Substrate 12 of the
`battery 10 comprises mica. A crystalline lithium metal oxide
`film may be used as the cathode film 18.
`17 Claims, 3 Drawing Sheets
`
`
`
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`

`

`US 6,632,563 B1
`Page 2
`
`OTHER PUBLICATIONS
`U.S. Provisional Patent Application entitled, “ Apparatus and
`Method for Rechargeable Batteries and for Making and
`Using Batteries”, filed Aug. 14, 2000, Ser. No. 06/225,134,
`Inventor: Jenson.
`U.S. Provisional Patent Application entitled, “Battery Hav
`ing Ultrathin Electrolyte”, filed Oct. 6, 2000, Ser. No.
`60/238,673; Inventor: Jensen, et al.
`Roh N-S, et al., “Effects of deposition condition on the ionic
`conductivity and structure of amorphous lithium phosphorus
`oxynitrate thin film' Scripta Materialia, Dec. 17, 1999, pp.
`43–49, vol. 42, No. 1, Elsevier, New York, NY, US.
`
`Neudecker, et al., “Lithium-Free Thin-Film Battery with
`In-Situ Plated Li Anode”, Journal of the Electrochemical
`Society, Issue No 147(2) 517-523 (2000).
`Donald M. Mattox, Handbook of Physical Vapor Deposition
`(PVD) Processing, Film Formation, Adhesion, Surface
`Preparation and Contamination Control, 1998, pp. 127-135
`and 343-364, Noyes Publications, Westwood, New Jersey,
`U.S.A.
`Bates, J.B., et al., “Preferred Orientation of Polycrystalline
`LiCoO Films” Journal of the Electrochemicial Society;
`Issue No.147 (1) pp. 59–70 (2000).
`* cited by examiner
`
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`

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`U.S. Patent
`
`Oct. 14, 2003
`
`Sheet 1 of 3
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`US 6,632,563 B1
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`U.S. Patent
`
`Oct. 14, 2003
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`Sheet 2 of 3
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`US 6,632,563 B1
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`Ameal Substrate
`
`100
`
`Load Substrate and
`pump down chamber
`
`Backfill chamber with Ar
`and 0 to 5 to 25 mTorr
`
`Operate magnetron sputering
`cathode at 1 to 20 Wlcm
`
`Deliver an ion-flux of 0.1 to
`5 mA/cm2 during deposition
`
`200
`
`300
`
`400
`
`500
`
`Establish a negative potential
`of 5 to 100 W on the substrate
`
`600
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`Maintain parameters to
`desired cathode thickness
`
`700
`
`---
`
`FIG. 2
`
`

`

`U.S. Patent
`
`Oct. 14, 2003
`
`Sheet 3 of 3
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`US 6,632,563 B1
`
`600
`500
`400
`300
`200
`100
`0
`15
`
`35
`
`40
`
`45
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`20
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`25
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`30
`Z 0–
`FIG. 4
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`12 14 1.6
`1
`0 02 04 06 0.8
`Capacity (mAh)
`FIG. 5
`
`1.8
`
`2
`
`

`

`1
`THIN FILM BATTERY AND METHOD OF
`MANUFACTURE
`
`US 6,632,563 B1
`
`BACKGROUND
`The invention relates to thin film batteries and methods of
`manufacture.
`A thin film battery typically comprises a Substrate having
`one or more thin films thereon, which may serve as, for
`example, current collectors, a cathode, an anode, and an
`electrolyte, that cooperate to generate a Voltage. The thin
`film batteries typically are less than about 400" of the
`thickness of conventional batteries. The thin films are typi
`cally formed by thin film fabrication processes, Such as for
`example, physical or chemical vapor deposition methods
`(PVD or CVD), oxidation, nitridation or electro-plating. The
`Substrate material is Selected to provide good dielectric
`properties and good mechanical Strength. Suitable Substrate
`materials may include for example, oxides Such as alu
`minium oxide and Silicon dioxide; metals. Such as titanium
`and StainleSS Steel; and SemiconductorS Such as Silicon.
`However, conventional Substrate materials often limit the
`ability of the battery to Store electrical energy to achieve
`high energy density or Specific energy levels. The energy
`density level is energy level per unit Volume of the battery.
`The Specific energy level is the energy level per unit weight
`of the battery. Conventional batteries typically achieve
`energy density levels of 200 to 350 Whr/l and specific
`energy levels of 30 to 120 Whr/l. However, it is desirable to
`have a thin film battery that provides higher energy density
`and Specific energy levels to provide more power per unit
`weight or Volume.
`The ability to achieve higher energy levels is also
`enhanced by forming a crystalline cathode film on the
`Substrate. The crystalline cathode film can also provide
`better charging and discharging rates. However, it is difficult
`to fabricate thin film batteries having crystalline cathode
`films on the substrate. Typically, the cathode is a thin film
`deposited on the Substrate in the amorphous or microcryS
`talline form, and thereafter, crystallized by annealing at high
`temperatures. For example, an amorphous or microcrystal
`line film of LiCoO is typically annealed at about 700° C. to
`obtain a crystalline LiCoO cathode film. However, the
`higher annealing temperature constrains the types of mate
`rials that may be used to form the other thin films on the
`Substrate. The other thin film materials should not, for
`example, Soften, melt, oxidize, or inter-diffuse at annealing
`temperatures. The annealing proceSS may also generate
`thermal stresses that arise from the difference in thermal
`expansion coefficient of the Substrate, cathode, and current
`collector, resulting in delamination or peeling off of the thin
`films or even the entire thin film battery structure. Thus,
`conventional methods are often deficient in their ability to
`fabricate the crystalline cathode film of the thin film battery.
`Thus it is desirable to have a thin film battery capable of
`providing relatively high energy density and Specific energy
`levels. It is also desirable to reduce the temperatures of
`fabrication of the crystalline thin film materials, especially
`in the fabrication of cathode comprising LiCoO.
`SUMMARY
`In one aspect, the present invention comprises a battery
`comprising first and Second electrodes on a Substrate that is
`less than 100 microns thick.
`In another aspect, the present invention comprises a thin
`film battery comprising a Substrate comprising mica and first
`and Second electrodes on the Substrate.
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`2
`In yet another aspect, the present invention comprises a
`method of manufacturing a battery comprising forming a
`Substrate comprising mica, and forming one or more films
`on the Substrate to generate or Store an electrical charge.
`In a further aspect, the present invention comprises a
`method of making a thin film battery comprising placing a
`Substrate in a chamber having a LiCoO target, introducing
`a process gas into the chamber, energizing the gas by
`applying a current at a power density level of from about 0.1
`to about 20 W/cm to the target, and exhausting the gas.
`In another aspect, the present invention comprises a
`Sputtering chamber comprising a fixture for holding a
`Substrate, a Sputtering target facing the Substrate, a gas outlet
`to provide a gas to the chamber, a pair of electrodes to
`energize the gas to Sputter the target, and a plurality of
`magnets about the Sputtering target, the magnets having
`different magnetic field Strengths.
`
`DRAWINGS
`These and other features, aspects, and advantages of the
`present invention will become better understood with refer
`ence to the following description, appended claims, and
`accompanying drawings, which illustrate embodiments of
`the present invention that may be used separately or in
`combination with one another, where:
`FIG. 1 is a schematic cross-sectional view of an embodi
`ment of a thin film battery according to the present inven
`tion;
`FIG. 2 is a flow chart of the method of fabricating a thin
`film battery according to another embodiment of the present
`invention;
`FIG. 3 is a schematic diagram of the structure of a
`magnetron Sputtering cathode apparatus according to the
`present invention;
`FIG. 4 is an X-ray diffraction pattern of an as-deposited
`LiCoO film showing that the film is highly crystalline and
`with a (110) preferred orientation; and
`FIG. 5 is a discharge curve of a thin film battery according
`to the present invention having a crystalline LiCoO cath
`ode.
`
`DESCRIPTION
`One embodiment of a battery 10 having features of the
`present invention is illustrated in FIG. 1. The battery 10 is
`formed on a Substrate 12 which can be an insulator, a
`Semiconductor, or a conductor. The Substrate 12 should also
`have Sufficient mechanical Strength to Support the thin films
`during processing or operational temperatures. For example,
`the Substrate 12 can comprise Silicon dioxide, aluminum
`oxide, titanium, or a polymer.
`In one embodiment of the present invention, which may
`be used by itself, or in combination with any of the other
`features or methods described herein, the Substrate 12 com
`prises a thickness of less than about 100 microns, and more
`preferably less than 25 microns. The thinner substrate 12
`reduces the total weight and Volume of the battery and yet
`is Sufficiently Strong to provide the desired mechanical
`Support for the battery Structure. A preferred Substrate mate
`rial comprises mica, which may be fabricated into a thin
`Substrate of less than 100 microns with good tensile Strength.
`Mica is typically a muscovite material, which is a layered
`Silicate with a typical Stoichiometry of KAlSiOo(OH).
`Mica typically has a flat six-sided monoclinical crystalline
`Structure with good cleavage properties in the direction of
`the large planar Surfaces. Because of this crystal Structure,
`
`

`

`3
`mica may be split into thin foils along its cleavage direction
`to provide thin substrates having surfaces 13 which are
`Smoother than most chemically or mechanically polished
`Surfaces, which is advantageous for the fabrication of thin
`films on the Substrate. Chemically, mica is stable and inert
`to the action of most acids, water, alkalies and common
`Solvents. Electrically, mica has good dielectric Strength, a
`uniform dielectric constant, and low electrical power loSS
`factors. Mica is also stable at high temperatures of up to 600
`C. By using mica, thin Substrates may be fabricated to
`provide lighter and smaller batteries with relatively higher
`energy density levels. Mica also provides good physical and
`chemical characteristics for processing of the thin films
`formed on the Substrate, in a CVD or PVD chamber, Such as
`for example, a magnetron Sputtering chamber.
`Referring to FIG. 1, a typical battery 10 includes a first
`adhesion layer 14 deposited on a Substrate 12 to improve
`adhesion of the other thin films formed on the Substrate 12.
`The adhesion layer 14 can comprise a metal Such as, for
`example, titanium, cobalt, aluminum, other metals, or a
`ceramic material Such as, for example, LiCoO, which may
`comprise a Stoichiometry of LiCoO. A first current collector
`16 is formed over the adhesion layer 14. The current
`collector 16 is typically a conductive layer which may
`comprise a non-reactive metal Such as Silver, gold, platinum
`25
`or aluminum. The first current collector 16 may also com
`prise the same metal as the adhesion layer 14 in a thickneSS
`that is sufficiently high to provide the desired electrical
`conductivity.
`A first electrode 18 comprising an electrochemically
`active material may be deposited over the first current
`collector 16. For example, the first electrode film 18 may
`comprise an amorphous Vanadium pentoxide, VOs, or one
`of Several lithium intercalation compounds that may be
`deposited in thin-film form, Such as crystalline TiS,
`LiMnO or LiCoO. In one exemplary embodiment, a
`crystalline LiCoO film is deposited upon the current col
`lector 16 by RF or DC magnetron sputtering to serve as the
`first electrode or cathode. An electrolyte film 20 is formed
`over the first electrode 18. The electrolyte film 20 may be,
`for example, an amorphous lithium phosphorus oxynitride
`film otherwise known as a LiponTM film, Dupont de
`Nemours, Wilmington, Del. An anode or second electrode
`22 is deposited over the electrolyte film 20 and a second
`current collector 24 is deposited on the Second electrode 22
`and the substrate 12. Further layers may be formed to
`provide additional protection.
`In yet another embodiment of the present invention,
`which also may be used by itself, or in combination with any
`of the other features or methods described herein, the first
`electrode film 18 comprises a crystalline lithium metal oxide
`film, such as a LiCoO film. The crystalline LiCoO film can
`be fabricated at low temperatures preferably below 600 C.
`by a PVD process, such as RF or DC magnetron sputtering
`with a high plasma density, as provided herein.
`FIG. 2 illustrates the method of making a thin film battery
`according to the present invention. In the initial preheating
`step, step 100, the substrate. 12 is heat treated to anneal the
`Substrate 12. The substrate 12 is heated to about 400 C. in
`air for about 10 minutes to clean the Surface 13 of the
`Substrate 12 by burning off organic materials which may be
`formed on the surface 13 of the substrate 12. Subsequently,
`the thin film layers of the battery are deposited on the
`substrate 12. One or more of the thin films may be adapted
`to generate or Store an electrical charge.
`In one method, the Substrate is placed in a magnetron
`PVD chamber 150 as shown in FIG. 3, which is pumped
`
`35
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`down to 1x10, Torr, step 200. A suitable substrate com
`prises an array of 35 mmx62 mm sheets of mica. The
`chamber 150 comprises walls 155, a gas supply 158 con
`nected to a gas distributor 160, a gas exhaust 165, and a
`power supply 170 to apply a power to a target 175. A
`Substrate fixture 180 with the Substrate 12 thereon is carried
`into the processing chamber 150 by a conveyor and posi
`tioned facing the target 175. The substrate holding fixture
`180 is electrically isolated from the chamber walls 155
`which are typically electrically grounded. The proceSS
`chamber 150 is separated from a loading chamber (not
`shown) by a slit valve (also not shown). The process
`chamber 150 typically comprises a volume of about 24 sq ft
`with dimensions of about 4"x6'x1'. The Sputtering targets
`175 are sized about 5"x25". The process gas distributor 160
`is provided for distributing process gas into the chamber
`150. A process gas, Such as for example, argon and oxygen,
`may be introduced into the chamber 150 to serve as the
`Sputtering gas. The Sputtering gas is maintained in the
`chamber 150 at a pressure of from about 5 to about 25
`mTorr, in step 300, and provided at a flow rate ratio of Ar/O
`of from about 1 to about 45.
`A high density plasma is generated in the chamber 150 by
`a magnetron Sputtering cathode 185. The plasma is formed
`over an area that is Sufficiently large to coat the entire
`substrate 12, for example, an area of about 8"xabout 25". In
`one version, the magnetron cathode 185 comprises central
`magnets 110 that provide a weaker magnetic field than the
`Surrounding peripheral magnets 120. Both the peripheral
`and central magnets, 110, 120 have a polarity of South facing
`the chamber 150 and north facing away from the chamber
`150. In this configuration, the magnetic field 130 generated
`by the magnets 120 is not confined to near the magnetron
`cathode surface 185. Instead, the magnetic field lines 130
`extend to near the substrate 12. Secondary electrons follow
`the magnetic field lines to near the Substrate Surface to create
`high-density plasma in this area. In one version, the magnets
`120 are arranged about a perimeter of the target 175. Thus,
`the distribution of plasma ions about the Substrate 12 may be
`controlled with the magnetic field 130.
`To deposit a film of LiCoO on the substrate 12, a target
`175 comprising LiCoO is installed in the chamber 150 and
`the magnetron-Sputtering cathode 185 is operated at a power
`density level of from about 0.1 to about 20 W/cm, step 400.
`In conjunction with operating the cathode 185, an ion flux of
`from about 0.1 to about 5 mA/cm is delivered to the
`substrate 12 upon which the LiCoO, film is being deposited,
`step 500. During deposition, a negative potential of 5 to 100
`V on the substrate 12 is established with respect to the
`plasma, step 600. The potential can be established either by
`using an external power Supply or by electrically floating the
`substrate holding fixture 180. The parameters of the depo
`Sition process are maintained until the desired film thickness
`is reached, step 700. The temperature of the substrate 12
`during the deposition process is estimated to be from about
`100 to about 200 C.
`In one version the as-deposited LiCoO film fabricated
`according to the present method comprises LiCoO which is
`crystalline with a strong (101) preferred orientation and with
`a small amount of (012) oriented grains. FIG. 4 shows a
`typical X-ray two theta diffraction pattern of the as-deposited
`LiCoO film showing that the film is highly crystalline and
`with a (101) preferred orientation. The substrate 12 was
`Slightly tilted when taking X-ray diffraction in order to
`SuppreSS the diffraction peaks from the mica Substrate to
`better reveal the property of the LiCoO film. It is believed
`that the crystalline material was deposited due to a combi
`
`

`

`S
`nation of plasma heating, oxygen activation and plasma
`enhanced nucleation and growth processes. The as deposited
`crystalline material was a good cathode material.
`Optionally, the cathode film formed on the substrate may
`be annealed to further improve the quality of the cathode
`film. The annealing Step was found to increase the battery
`capacity by 10 to 20%, increase the charge and discharge
`current by more than 50%, and improve the resistance to
`moisture. These attributes arise from the elimination of point
`defects and the reduction of electrical contact resistances in
`the cathode material.
`Under lower gas pressure levels of about 5 mTorr, the
`preferred orientation changes to (012) and (104). The (012)
`and (104) oriented material can still be used as cathode,
`however, with Smaller energy capacity compared to the
`(101) oriented material. The annealing process is typically
`performed at a low temperature of from about 150 to about
`600° C.
`FIG. 5 is a typical discharge curve of a 15 cm thin film
`battery of the present invention. The battery comprised a 10
`m-thick mica Substrate with a crystalline LiCoO cathode
`layer that is close to 2 um. The capacity of the battery, as
`shown in FIG. 5, is about 1.9 mAh. Thus, the capacity of the
`cathode is calculated to be 0.07 mAh/cm/um, which is close
`to the theoretical number for crystalline LiCoO. The cut off
`voltage of this battery is well defined and at 3.7 V. The
`energy density and Specific energy of this thin film battery,
`including both the cell and the substrate, is about 340 wh/l
`and 105 wh/kg, respectively. It is expected that an energy
`density of more than 700 wh/1 and a specific energy of more
`than 250 wh/kg can be achieved by fabricating the battery
`cell on both front and back side of a mica Substrate. The
`discharge current of the battery was about 2 mA.
`It will be understood that numerous modifications and
`Substitutions can be made to the described exemplary
`embodiments of the present invention without departing
`from the scope of the invention. For example, thin film
`electronic devices other than batteries may be fabricated
`using the described Substrate. Also, the battery can include
`other combinations of metal, nonmetal and dielectric layers
`and in a different order than that described herein.
`Accordingly, the exemplary embodiments are intended for
`the purpose of illustration and not as a limitation.
`What is claimed is:
`1. Abattery comprising first and Second electrodes having
`an electrolyte therebetween, one of the electrodes compris
`ing a crystalline lithium metal oxide film, and the electrodes
`and electrolyte being Supported by a Substrate comprising a
`mica foil that is less than about 100 microns thick.
`2. A battery according to claim 1 wherein the Substrate is
`less than about 25 microns thick.
`3. A battery according to claim 1 comprising an adhesive
`layer between the Substrate and a current collector.
`4. A battery according to claim 1 wherein the electrolyte
`comprises amorphous lithium phosphorus Oxynitride.
`5. A thin film battery comprising:
`a Substrate comprising mica;
`first and Second electrodes Supported by the Substrate, one
`of the electrodes comprising a crystalline lithium metal
`oxide film; and
`an electrolyte between the electrodes, whereby the thin
`film battery is capable of Storing electrical energy.
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`6
`6. A battery according to claim 5 wherein the substrate
`comprises a thickness of less than about 100 microns.
`7. A battery according to claim 6 wherein the substrate
`comprises a thickness of less than about 25 microns.
`8. A battery according to claim 5 comprising an adhesive
`layer between the Substrate and a current collector.
`9. A thin film battery comprising:
`an anode film;
`a cathode film comprising crystalline lithium metal oxide;
`an electrolyte film between the anode and cathode films,
`and
`an annealed mica Substrate to Support the films,
`whereby the anode film, cathode film and electrolyte film
`cooperate to Store electrical energy.
`10. A battery according to claim 9 wherein the mica
`substrate comprises a thickness of less than about 100
`microns.
`11. Abattery according to claim 9 comprising an adhesion
`layer on the mica Substrate.
`12. A battery according to claim 9 further comprising an
`anode current collector film in contact with the anode film,
`and a cathode current collector film in contact with the
`cathode film.
`13. A battery according to claim 9 wherein the cathode
`film comprises crystalline LiCoO.
`14. A battery according to claim 9 wherein the electrolyte
`film comprises amorphous lithium phosphorus oxynitride.
`15. A thin film battery comprising:
`an anode current collector film;
`a cathode current collector film;
`an anode film contacting the anode current collector film;
`a cathode film contacting the cathode current collector
`film, the cathode film comprising crystalline LiCoO,
`an electrolyte film between the anode and cathode films,
`the electrolyte film comprising amorphous lithium
`phosphorous oxynitride;
`a mica foil to Support the films, the mica foil having a
`preheated Surface from which organic materials are
`burnt off, and
`an adhesion layer on the preheated Surface of the mica foil
`and contacting the cathode current collector film,
`whereby the anode current collector film, cathode current
`collector film, anode film, cathode film and electrolyte film
`cooperate to Store electrical energy.
`16. A battery according to claim 15 wherein the mica foil
`comprises a thickness of less than about 100 microns.
`17. A thin film battery comprising:
`a mica foil;
`an adhesion layer on the mica foil;
`a cathode current collector film on the adhesion layer;
`a cathode film contacting the cathode current collector
`film, the cathode film comprising a crystalline lithium
`metal oxide film;
`an electrolyte film on the cathode film; and
`an anode film over the electrolyte film,
`whereby the cathode current collector film, cathode film,
`electrolyte film and anode film cooperate to Store electrical
`energy.
`
`