DETAILED ACTION
Claims 1-36 are presented for examination, wherein claims 1, 12, 14-15, and 23 are currently amended; and, claims 6-7, 9-11, 16-22, and 24-36 are withdrawn, and further the subject matter of lithium-metal batteries, sodium-ion batteries, and sodium-metal batteries, with related compositions and anodes thereof; particulate not preloaded with said lithium or sodium, and related battery and components thereof; form of said lithium-/sodium-attracting metal as coating having a thickness from 0.5 nm to 10 µm; graphene sheets containing single layer graphene, which is 1 layer; said graphene sheets contain pristine graphene material having essentially zero % of non-carbon elements; and, said binder or matrix material being an electron-conducting material are withdrawn.
The objections to claims 14-15 are withdrawn, as a result of the amendments to said claims.
The nonstatutory double patenting rejection of claims 1-3 and 15 over U.S. 10,170,749 is held in abeyance, as requested in the February 9, 2022 filing.
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
Claims 1-3, 12-13, 15, and 23 are rejected under 35 U.S.C. 103 as being unpatentable over Zhamu et al (US 2012/0064409) in view of Zhamu et al (US 2017/0352868, hereinafter the “‘868 application”).
Regarding newly amended independent claim 1, Zhamu teaches a plurality of secondary particles/particulates for use as an anode active material in a lithium-ion battery, wherein said secondary particle/particulate is a composite of a plurality of graphene sheets and a plurality of primary anode active material particles, such as Si, Ge, Sn, Pb, Sb, Bi, Zn, Al, Ti, Ni, Co, or Cd, and alloys thereof with other elements, but not limited thereto, wherein said graphene sheets embrace and protect said primary active material particles (e.g. ¶¶ 0002, 39-48, 56, 62-65, 70-71, 75-77, 109-110, and 115 plus e.g. Figures 3, 4A-C, and 7B), reading on “powder mass comprising multiple metal-containing graphene balls or particulates as an anode active material for a lithium battery…,” said secondary particles/particulates comprising:
(1a) said secondary particle/particulate is said composite including said plurality of graphene sheets, wherein said graphene sheets embrace and protect said primary active material particles (e.g. supra), wherein said graphene sheets may be nano-graphene platelets (hereinafter “NGP”) that favorably has a thickness of less than 10 nm, i.e. less than 10 layers of graphene sheets, and a length, width, or diameter of less than 10 µm, wherein said secondary particles/particulates may have an average size of e.g. 10 µm; and, a broader teaching provides said secondary particles/particulates are “larger in average size” than said primary particles, which have a size smaller than 10 µm (e.g. ¶¶ 0055, 61, 71-72, and 76-78), establishing a prima facie case of obviousness of the claimed range, see also e.g. MPEP § 2144.05(I), reading on the previously amended limitation “at least one of said graphene balls or particulates comprising (a) a plurality of graphene sheets, each having a length or width from 5 nm to 100 µm and forming into said particulate….,” see also instant specification, at ¶¶ 0013 and 67; alternatively, the dimensions of said graphene sheets within said FLG does not patentably distinguish the instant invention, e.g. MPEP § 2144.04(IV)(A); and,
said broader teaching provides said secondary particles/particulates are “larger in average size” than said primary particles, which have said size smaller than 10 µm, indicates said secondary particles/particulates may have an average particle size of 10 µm or larger, establishing a prima facie case of obviousness of one option for the claimed diameter, see also e.g. MPEP § 2144.05(I), reading on the newly amended, previously amended limitation “at least one of said graphene balls or particulates comprising (a) a plurality of graphene sheets…forming into said particulate having a diameter of 100 nm or 20 µm;” alternatively, the dimensions of said particulate do not patentably distinguish the instant invention, e.g. MPEP § 2144.04(IV)(A), for example, the expressly taught secondary particles/particulates having said average size of e.g. 10 µm is within the instantly provided range of “100 nm to 20 µm” (instant specification, at e.g. ¶¶ 0013 and 67, emphasis added), see also infra, the endpoints of said range are the newly amended claimed diameters of the particulate “100 nm or 20 µm,” see e.g. infra.
SUMMARY…
[0013] In certain embodiments, the disclosure provides a powder mass comprising multiple metal-containing graphene balls or particulates as an anode active material for a lithium battery or sodium battery, the graphene ball or particulate comprising (a) a plurality of graphene sheets, each having a length or width preferably from 5 nm to 100 μm and forming into the ball or particulate having a diameter from 100 nm to 20 μm and (b) a lithium-attracting metal or sodium-attracting metal in a form of particles or coating having a diameter or thickness from 0.5 nm to 10 μm and in physical contact with the graphene sheets, wherein the metal is selected from Au, Ag, Mg, Zn, Ti, Na, K, Al, Fe, Mn, Co, Ni, Sn, V, Cr, an alloy thereof, or a combination thereof and is in an amount of 0.1% to 95% of the total particulate weight (more typically from 0.1% to 30%). The graphene ball or particulate can be substantially spherical, ellipsoidal, slightly elongated, or irregular in shape.
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DESCRIPTION OF THE PREFERRED EMBODIMENTS
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[0067] We have discovered a highly dendrite-resistant or dendrite-free, graphene ball-based anode configuration for a Li metal cell or Na metal cell that exhibits a high energy, high power density, and stable cycling behavior. In certain embodiments, the disclosure provides a powder mass comprising multiple metal-containing graphene balls or particulates as an anode active material for a lithium battery or sodium battery, the graphene ball or particulate (as illustrated in FIG. 3) comprising (a) a plurality of graphene sheets, each having a length or width from 5 nm to 100 μm and forming into the ball or particulate having a diameter from 100 nm to 20 μm and (b) a lithium-attracting metal or sodium-attracting metal in a form of particles or coating having a diameter or thickness from 0.5 nm to 10 μm and in physical contact with the graphene sheets, wherein the metal is selected from Au, Ag, Mg, Zn, Ti, Na, K, Al, Fe, Mn, Co, Ni, Sn, V, Cr, an alloy thereof, or a combination thereof and is in an amount of 0.1% to 95% of the total particulate weight (more typically from 0.1% to 30%). The graphene ball or particulate can be substantially spherical, ellipsoidal, slightly elongated, or irregular in shape.
(Instant specification, at e.g. ¶¶ 0013 and 67, emphasis added); and,
(2) said primary anode active material particles may be composed of plurality of primary anode active material particles, such as Si, Ge, Sn, Pb, Sb, Bi, Zn, Al, Ti, Ni, Co, or Cd, and alloys thereof with other elements, but not limited thereto (e.g. supra), wherein said primary anode active material particles have a size smaller than 10 μm, preferably smaller than 100 nm (e.g. ¶¶ 0039, 41, 48, 71, and 75),
wherein said graphene is in an amount of at least 0.01% by weight, but typically much lower than 99% and said primary anode active material particles is in an amount of at least 0.1% by weight, based on the total weight of the particulate (e.g. ¶0039); and, wherein said graphene sheets embrace and protect said primary active material particles to form secondary particles/particulates (e.g. supra),
severably establishing a prima facie case of obviousness of the claimed ranges, see also e.g. MPEP § 2144.05(I), reading on the previously amended limitation “at least one of said graphene balls or particulates comprising…(b) a lithium-attracting metal…in a form of particles…having a diameter…from 0.5 nm to 10 μm and in physical contact with the graphene sheets…and is in an amount of 0.1% to 95% of the total particulate weight,” but does not expressly teach the previously amended limitation “the metal is selected from Na, K, Cr, an alloy thereof, or a combination thereof….”
However, the ‘868 application teaches an integral 3D graphene-carbon-metal hybrid foam used as an anode, said hybrid foam composed of multiple pores, pore walls, and a lithium-attracting metal nanoparticles residing in said pores, wherein
(1) said pore walls containing few-layer graphene sheets (hereinafter “FLG” sheets) have 2-10 layers of stacked graphene planes and said FLG sheets each having a length or width greater than 20 nm and often greater than 1 µm; and,
(2) said lithium-attracting metal selected from Zn, Ti, Na, K, Al, Co, Ni, Sn, Cr, or an alloy thereof, said metal nanoparticles in an amount of 0.1% to 50% of the total hybrid foam weight or volume, wherein said lithium-attracting metal are lithiated as lithium ions are transferred to the anode
(e.g. ¶¶ 0040, 43, 49, 72, 77, 100, 102, 124-125, 135, 156, 159-160, and 188), wherein it is understood that by being lithiated, said lithium-attracting metals (Zn, Ti, Na, K, Al, Co, Ni, Sn, Cr, or an alloy thereof) are active materials, see also e.g. Zhamu, which teaches Zn, Ti, Al, Co, Ni, Sn, and alloys thereof are anode active materials (e.g. ¶¶ 0011, 41, and 75).
As a result, it would have been obvious to a person of ordinary skill in the art to substitute the Na, K, Cr, or alloy thereof composition of the ‘868 for the anode active material composition of Zhamu (e.g. Zn, Ti, Al, Co, Ni, Sn, and alloys thereof), since the ‘868 application teaches they are equivalent compositions capable of lithiation.
Zhamu as modified reading on “a lithium-attracting metal…in a form of particles…having a diameter…from 0.5 nm to 10 μm and in physical contact with the graphene sheets, wherein the metal is selected from Na, K, Cr, an alloy thereof, or a combination thereof and is in an amount of 0.1% to 95% of the total particulate weight.”
Regarding claim 2, Zhamu as modified teaches said plurality of particulates of claim 1, wherein Zhamu teaches said graphene sheets may be NGP that favorably has a thickness of less than 10 nm, i.e. less than 10 layers of graphene sheets (e.g. supra), wherein such graphene sheet containing less than 10 layers of graphene sheets are few-layer graphene (hereinafter “FLG”), reading on “multiple graphene sheets contain…few-layer graphene,” establishing a prima facie case of obviousness of the claimed range, see also e.g. MPEP § 2144.05(I), reading on “said few-layer graphene sheets have 2-10 layers of stacked graphene planes…;” and further, said FLG NGP may be composed of graphene having an oxygen content of less than 5 wt% (e.g. ¶¶ 0053 and 107-108, compared with instant specification, at e.g. ¶¶ 0028, 96, and 116), wherein graphene including oxygen would not be pristine, establishing a prima facie case of obviousness of the claimed range, see also e.g. MPEP § 2144.05(I), reading on “said…few-layer graphene sheets contain…a non-pristine graphene material having 0.001% to 25% by weight of non-carbon elements,” but does not expressly teach said FLG NGP having the property of “inter-plane spacing d002 from 0.3354 nm to 0.6 nm as measured by X-ray diffraction.” However, Zhamu teaches a substantially identical composition (e.g. supra, compared with instant specification, at e.g. ¶¶ 0014 and 116), establishing a prima facie case of obviousness of said property, see also e.g. MPEP § 2112.01.
Regarding claim 3, Zhamu as modified teaches said plurality of particulates of claim 2, wherein Zhamu teaches said FLG NGP may be composed of graphene having an oxygen content of less than 5 wt% (e.g. supra), reading on “said non-pristine graphene is selected from graphene oxide, reduced graphene oxide, graphene fluoride, graphene chloride, graphene bromide, graphene iodide, hydrogenated graphene, nitrogenated graphene, doped graphene, chemically functionalized graphene, or a combination thereof.”
Regarding claim 15, Zhamu as modified teaches said plurality of particulates of claim 1, wherein Zhamu teaches said FLG NGP of said particulates are composed of less than 10 layers of graphene sheets having an oxygen content of less than 5 wt% (e.g. supra), but does not expressly teach the properties of “said graphene ball or particulate, when measured without said metal, has a density from 0.005 to 1.7 g/cm3 and a specific surface area from 50 to 2,630 m2/g.”
However, Zhamu teaches a substantially identical FLG NGP (e.g. supra, compared with instant specification, at e.g. ¶¶ 0027 and 117), establishing a prima facie case of obviousness of said property, see also e.g. MPEP § 2112.01.
Regarding claims 12-13 and 23, Zhamu and the ‘868 application are applied for the reasons provided supra, with the following modifications.
Still regarding newly amended independent claim 12, Zhamu further teaches said particulate may further comprise therein a carbon or graphite material in electronic contact with said anode active material and said graphene sheet; said carbon or graphite material may be coated on or in contact with at least one of said anode active material particles and said graphene sheet, wherein said carbon or graphite material may be fine expanded graphite particle (e.g. ¶0050), wherein the claimed shape “flake” does not patentably distinguish the instant invention, see e.g. MPEP § 2144.04(IV)(B), noting there does not appear to be significance, see e.g. instant specification, at e.g. ¶¶ 0022, 81-82, and 114, reading on the previously amended limitation “at least one of the graphene balls or particulates further contains an electron-conducting material selected from an expanded graphite flake, an electron-conducting polymer, or combination thereof.”
Still regarding claim 13, Zhamu as modified teaches the plurality of particulates of claim 12, wherein said carbon or graphite material in electronic contact within said particulate may be said fine expanded graphite particle (e.g. supra), so the option of electron-conducting polymer in claims 12-13, including the instant limitation “said electron-conducting polymer is selected from polyaniline, polypyrrole, polythiophene, polyfuran, polyacetylene, a bi-cyclic polymer, a sulfonated derivative thereof, or a combination thereof” does not patentably distinguish the instant invention from the art.
Still regarding newly amended independent claim 23, Zhamu teaches said lithium-ion battery comprising said plurality of secondary particles/particulates for use as said anode active material (e.g. supra), reading on “lithium-ion battery,” said battery comprising:
(1) an anode (e.g. ¶¶ 0056-58, 71 and 109-110), reading on “an anode,”
(2) a cathode (e.g. ¶¶ 0056-58, 81 and 109-111), reading on “a cathode,”
(3) an electrolyte in contact with both said anode and said cathode, said electrolyte solvating lithium ions therein (e.g. ¶¶ 0056, 70-71, 109, and 115-118), reading on “an electrolyte in ionic contact with said anode and said cathode,”
wherein said anode comprises said plurality of secondary particles/particulates as said anode active material (e.g. supra), reading on “said anode comprises a powder mass,”
wherein said cathode active material may be selected from the group consisting of lithium cobalt oxide, lithium nickel oxide, lithium manganese oxide, lithium vanadium oxide, lithium-mixed metal oxide, lithium iron phosphate, lithium manganese phosphate, lithium vanadium phosphate, lithium mixed metal phosphates, and combinations thereof (e.g. ¶¶ 0111-112); and, said electrolyte in physical contact with both said anode and said cathode, said electrolyte solvating lithium ions (e.g. supra), reading on “said cathode comprises a lithium-containing cathode active material,” which is capable of the property “releases lithium ions into said electrolyte when the battery is charged,” see also e.g. MPEP §§ 2114 and 2112.01;
further, said electrolyte in contact with both said anode and said cathode, said electrolyte solvating lithium ions (e.g. supra), which is capable of the property “the released lithium ions move to the anode,” see also e.g. MPEP §§ 2114 and MPEP § 2112.01; and,
further, said Na, K, Cr, or alloy thereof are lithiated as lithium ions are transferred to the anode (e.g. supra), reading on the limitation “the released lithium ions…react with said metal or form an alloy with said metal in the anode.”
Claims 4-5, 8, and 14 are rejected under 35 U.S.C. 103 as being unpatentable over Zhamu et al (US 2012/0064409) in view of Zhamu et al (US 2017/0352868, hereinafter the “‘868 application”), as provided supra, and further in view of Zhamu et al(US 2017/0288211, hereinafter the “‘211 application”).
Regarding claims 4-5, 8, and 14, Zhamu as modified teaches said plurality of particulates of claim 1, wherein Zhamu teaches said particulate may further comprise therein a carbon or graphite material in electronic contact with said anode active material and said graphene sheet, wherein said carbon or graphite material may be coated on or in contact with at least one of said anode active material particles or said graphene sheet, wherein said carbon or graphite material is selected from polymeric carbon, amorphous carbon, chemical vapor deposition carbon, coal tar pitch, petroleum pitch, meso-phase pitch, carbon black, coke, acetylene black, activated carbon, fine expanded graphite particle with a dimension smaller than 100 nm, artificial graphite particle, natural graphite particle, or a combination thereof (e.g. ¶0050), but does not expressly teach the limitations of claims 4-5, 8, and 14, which depend from claim 1, wherein claim 1 was previously amended to delete the previously amended, previously added limitation, “at least one of the graphene balls or particulates further comprises an intrinsically conducting polymer selected from polyacetylene, a sulfonated derivative thereof, or a combination thereof.”
However, the ‘211 application teaches an anode active material for use in lithium secondary batteries, said anode active material in the form of a plurality of active material particles (e.g. ¶¶ 0001, 15, and 46-53),
wherein said active material particles are encapsulated by a thin layer of elastomeric material that has a lithium ion conductivity no less than 10−7 S/cm at room temperature and an encapsulating shell thickness from 1 nm to 100 nm, wherein the coating entirely covers the active material particle to protect the active material from directly contacting the electrolyte and further reduce the effects of expansion/contraction during cycling, but also where the thickness affects the ion-conductivity to the active material (e.g. ¶¶ 0016, 30, 46-49, 56-57, 61, and 99),
wherein said elastomeric material may be composed of e.g. natural polyisoprene (e.g. cis-1,4-polyisoprene natural rubber), synthetic polyisoprene, polybutadiene (butadiene rubber), chloroprene rubber, polychloroprene, butyl rubber, including halogenated butyl rubbers, styrene-butadiene rubber, nitrile rubber, ethylene propylene rubber, ethylene propylene diene rubber, epichlorohydrin rubber, polyacrylic rubber, silicone rubber, fluorosilicone rubber, fluoroelastomers, perfluoroelastomers, polyether block amides, chlorosulfonated polyethylene, ethylene-vinyl acetate, thermoplastic elastomers, protein resilin, protein elastin, ethylene oxide-epichlorohydrin copolymer, polyurethane, urethane-urea copolymer, and combinations thereof (e.g. ¶¶ 0025 and 61);
wherein said elastomeric material may contain a mixture or blend of an elastomer and an electron-conducting polymer selected from polyaniline, polypyrrole, polythiophene, polyfuran, a bi-cyclic polymer, derivatives thereof (e.g. sulfonated versions), or a combination thereof (e.g. ¶0028); and,
wherein said elastomeric material may further contain a lithium ion-conducting additive dispersed in said elastomer matrix material, wherein said lithium ion-conducting additive may be Li2CO3, Li2O, Li2C2O4, LiOH, LiX, ROCO2Li, HCOLi, ROLi, (ROCO2Li)2, (CH2OCO2Li)2, Li2S, LixSOy, or a combination thereof, wherein X = F, Cl, I, or Br, R = a hydrocarbon group, x = 0-1, y = 1-4 (e.g. ¶0063).
As a result, it would have been obvious to use the encapsulating shell of the ‘211 application to entirely encapsulate the primary anode active material particles of Zhamu as modified, since the ‘211 application teaches said encapsulating shell by entirely coating active material particle protects the active material from directly contacting electrolyte and/or reduces the effects of expansion/contraction during cycling.
Still regarding previously amended claim 4, Zhamu as modified teaches the plurality of particulates of claim 1, wherein said taught elastomeric material compositions are severably known binder materials, so would be expected to bind together the plurality of graphene sheets, which embrace and protect said primary active material particles that are coated with said encapsulating shell,
wherein Zhamu teaches in said secondary particles/particulate, said graphene is in an amount of at least 0.01% by weight, but typically much lower than 99% and said primary anode active material particles is in an amount of at least 0.1% by weight, all based on the total weight of the particulate (e.g. supra), so the balance may be considered to be said elastomeric material, establishing a prima facie case of obviousness of the claimed range, see also e.g. MPEP § 2144.05(I), “0.01% to 40% by weight of a binder or matrix material,” reading on the previously amended limitation “at least one of said graphene balls or particulates further comprises 0.01% to 40% by weight of a binder or matrix material that holds said multiple graphene sheets together as a composite graphene ball.”
Still regarding claims 5 and 8, Zhamu as modified teaches the plurality of particulates of claim 4, wherein said elastomeric material may further contain said lithium ion-conducting additive dispersed in said elastomer matrix material, wherein said lithium ion-conducting additive may be Li2CO3, Li2O, Li2C2O4, LiOH, LiX, ROCO2Li, HCOLi, ROLi, (ROCO2Li)2, (CH2OCO2Li)2, Li2S, LixSOy, or said combination thereof, wherein X = F, Cl, I, or Br, R = a hydrocarbon group, x = 0-1, y = 1-4 (e.g. supra), reading on “said binder or matrix material comprises an…lithium ion-conducting material” (claim 5) and “said lithium ion-conducting material is selected from Li2CO3, Li2O, Li2C2O4, LiOH, LiX, ROCO2Li, HCOLi, ROLi, (ROCO2Li)2, (CH2OCO2Li)2, Li2S, LixSOy, or a combination thereof, wherein X = F, Cl, I, or Br, R = a hydrocarbon group, 0 < x ≤ 1, 1 ≤ y ≤ 4” (claim 8).
Still regarding previously amended 14, Zhamu as modified teaches said plurality of particulates of claim 1, wherein Zhamu teaches said particulates are uses as a lithium-ion secondary battery anode active material, wherein said particulate is formed of said plurality of graphene sheets embracing and protecting said primary active material particles; and, said primary anode active material particles composed of Mn; and further, Mn is an equivalent anode active material to at least one of e.g. Si, Ge, Sn, Pb, Sb, Bi, Zn, Al, Ni, Co, Ti, and Cd (e.g. supra), but does not expressly teach the previously amended limitation “the graphene ball or particulate further comprises lithium metal…residing in the ball or in physical contact with the lithium-attracting metal…to form a lithium-preloaded or sodium-preloaded graphene particulate.”
However, the ‘211 application teaches said anode active material for use in lithium secondary batteries, said active material particles may be composed of e.g. Zn, Ti, or Co; alloys thereof with other elements; prelithiated versions thereof; particles of Li, Li alloy, or surface-stabilized Li having at least 60% by weight of lithium element therein; particles of Li or Li alloy (Li alloy containing from 0.1% to 10% by weight of e.g. Zn, Ti, or Co, element; and, combinations thereof (e.g. supra).
As a result, it would have been obvious to additionally incorporate said particles of Li, Li alloy, or surface-stabilized Li of the ‘211 application with said Na, K, and/or Cr primary anode active material particles of Zhamu as modified, since the ‘211 application teaches they are equivalent anode active materials to at least one of e.g. Zn, Ti, and Co, which are in turn equivalent anode active materials to Na, K, and/or Cr, wherein said plurality of graphene sheets embracing and protecting said primary active material particles, reading on said limitation, see also e.g. MPEP § 2144.06.
Response to Arguments
Applicant’s arguments filed December 16, 2025 have been fully considered but they are not persuasive. The applicant alleges the art does not teach the newly amended limitations of claims 1, 12, or 23, from which the other claims depend (Remarks, at e.g. pp. 8-9).
In response, the examiner respectfully refers supra.
Conclusion
Applicant's amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a).
A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to YOSHITOSHI TAKEUCHI whose telephone number is (571)270-5828. The examiner can normally be reached M-F, 8-4.
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/YOSHITOSHI TAKEUCHI/Primary Examiner, Art Unit 1723