Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Election/Restrictions
Applicant’s election of Group I (claims 1-14 and 16) in the reply filed on 10/20/25 is acknowledged. Because applicant did not distinctly and specifically point out the supposed errors in the restriction requirement, the election has been treated as an election without traverse (MPEP § 818.01(a)).
Claims 15 and 17-20 withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected inventions, there being no allowable generic or linking claim. Election was made without traverse in the reply filed on 10/20/25.
Claim Rejections - 35 USC § 102/103
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 (i.e., changing from AIA to pre-AIA ) 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 following is a quotation of the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
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 (i.e., changing from AIA to pre-AIA ) 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 following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
Claim(s) 1, 4-6, and 8-12 is/are rejected under 35 U.S.C. 102(a) (1) as anticipated by or, in the alternative, under 35 U.S.C. 103 as obvious over Oladeji (US 2012/0137508; provided in 9/9/24 IDS; hereafter Oladeji).
As anticipated:
Claim 1: Oladeji teaches a method for making a lithium salt film (cathode material film, such as LiMPO4), (See, for example, abstract, [0060-0061], [0082]) the method comprising:
heating a substrate (see, for example, [0023], [0030], [0037], examples);
while heating, spraying a mixture onto the substrate to form a precursor film (See, for example, [0023], [0030], [0037] examples), the mixture comprising:
a first precursor comprising a lithium ion (such as lithium salt of acetate, sulfate, chloride, citrate, or nitrate) (See, for example, [0062]);
a second precursor comprising an anion (such as various acids, metal salts, ammonia, phosphoric acid, etc) (see, for example, [0062], ;
and a solvent (such as water) (see, for example, [0060]);
and annealing the precursor film to form the lithium salt film having a thickness of about 2 micron (see, for example, [0066] ~1 micron / min for 2 minutes, or [0068]), or 10 micron (see, for example, [0072], [0077], wherein deposition proceeds at ~1 micron / minute at 10 minutes);
wherein: the lithium salt film comprises the lithium ion and the anion (such as LiMPO4) (See, for example, [0061], or [0082]);
and while annealing, the precursor film has a temperature of 400° C or 700° C (See, for example, [0066], [0073], [0078]).
Alternatively, as obviated:
Claim 1: refer the rejection of claim 1 over Oladeji above, although no singular exemplary embodiment was provided for the LiMPO4 lithium salt film system, it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated the components and conditions as articulated above since a reasonable expectation of success exists from choosing the specific taught species from explicitly taught lists. Further when the species is clearly named, the species claim is anticipated (rendered obvious) no matter how many other species are additionally named. Ex parte A 17 USPQ2d 1716 (Bd. Pat. App. & Inter. 1990).
Claim 4: Oladeji further teaches wherein the solvent comprises water, or alcohol (methanol, ethanol, methoxypropanol) (see, for example, [0060], [0062] examples).
Claim 5: Oladeji further teaches wherein the first precursor comprises at least one of lithium acetate, or lithium nitrate (see, for example, [0062], examples).
Claim 6: Oladeji further teaches wherein the second precursor comprises at least one of a sulfate ion, a hydroxide ion, nitrate ion, nitride ion, a phosphate ion, or a chloride ion (see, for example,
Claim 8: Oladeji further teaches wherein its film comprises at least one of lithium phosphate such as LiMPO4) (See, for example, [0061], [0083].
Claim 9: Oladeji further teaches wherein the substrate is a solid substrate comprising at least one of a metal, a metal oxide, a metal alloy, carbon, silicon (see, for example, [0060], and examples, such as stainless steel).
Claim 10: Oladeji further teaches depositing a capping layer on a surface of the lithium salt film (such as electrolyte, separator, anode, current collector, leads, or cell walls) (See, for example, [0032-33], [0041-45]).
Claim 11-12: Oladeji further teaches wherein: the mixture further comprises a third precursor comprising a second metal ion (such M = Fe, Co, Ni, Mn etc) and the lithium salt film further comprises the second metal ion (such as LiMPO4) (see, for example, [0061-62], [0082]).
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 (i.e., changing from AIA to pre-AIA ) 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 following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
Claim(s) 2-3 is/are rejected under 35 U.S.C. 103 as being unpatentable over Oladeji as applied to claim 1 above, and further in view of Badding et al (US 2014/0084503; hereafter Badding).
Claim 2: Oladeji teaches the method of claim 1 wherein the lithium ion is dissolved in the solvent (See, for example, [0060-0062]), but does not explicitly teach the dissolution is at a lithium ion concentration at a stoichiometric excess greater than a stoichiometric amount of the lithium ion in the lithium salt film. Badding teaches a method of forming LiMPO4 type lithium salt films by spraying (See, for example, abstract). Badding further teaches wherein lithium volatility is well recognized in the art, and to compensate for this volatility the preparation of precursor solutions with an excess of Li with respect to desired stoichiometry is performed (See, for example, [0035]). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a concentration of the lithium ion in the solvent at a stoichiometric excess greater than a stoichiometric amount of the lithium ion in the lithium salt film as it would predictably compensate for Li volatilization.
Claim 3: Badding has further taught wherein the stoichiometric excess is 10%-20% (see, for example, [0037]).
Claim(s) 7 is/are rejected under 35 U.S.C. 103 as being unpatentable over Oladeji as applied to claim 6 above, and further in view of Barker et al (US 2002/0039687; hereafter Barker) and Tang et al (CN1785823; citations directed to machine translation provided herein, hereafter Tang).
Claim 7: Oladeji teaches the method of claim 1 above, further teaching wherein the film formed can comprise lithium battery electrode material such as LiMPO4 (See, for example, [0060-0061], [0082]). And wherein the precursor can comprise sulfate ions (sulfuric acid) and ammonia (See, for example, [0062]). But it does not explicitly teach wherein the second precursor comprises ammonium sulfate. Barker similarly teaches a method of forming lithium battery electrode material, further of LiMPO4 typing (See, for example, [0006]). Baker further teaches it is known to replace phosphorus with sulfur in such structures, and such replacement is performed via using ammonium sulfate in the starting materials (See, for example, [0016]). Tang similarly is directed to a method of forming lithium battery electrode material, further of LiMPO4 typing (See, for example, [0007]). Tang further teaches wherein replacement of P with S is found to improve basic electrical properties of the electrode material giving it higher discharge capacity and good battery cycle performance (See, for example, [0007]). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to the second precursor comprise ammonium sulfate as such an addition would predictably allow for sulfur replacement of phosphorus within the LiMPO4 electrode material resulting in improved basic electrical properties of the electrode material giving it higher discharge capacity and good battery cycle performance.
Claim(s) 13 is/are rejected under 35 U.S.C. 103 as being unpatentable over Oladeji as applied to claims 1 and 11 above, and further in view of Nagayama et al (US 2003/0013017; hereafter Nagayama).
Claim 13: Oladeji teaches the method of claim 1 above, further teaching wherein the film formed can comprise lithium battery electrode material (such as LiMPO4, and various lithium mixed metal salt systems) (See, for example, [0060-0061], [0082], further wherein M is Co). And wherein the metal precursors can comprise metal sulfates (See, for example, [0062]). But it does not explicitly teach wherein the second metal ion of the third precursor comprises calcium, as calcium sulphate. Nagayama similarly teaches a method of forming lithium battery electrode material, further of mixed metal salt typing (See, for example, abstract). Nagayama further teaches wherein suppression of increase in battery thickness due to repeated charge / discharge cycles, and thus improve discharge capacity and thermal stability of a battery can be improved by partially replacing lithium and metal elements within the electrode with a element M, further Calcium (See, for example, [0008-00011], [0017-[0020]). Nagayama similarly teaches wherein the incorporation of calcium can be predictably achieved by using calcium sulfate (See, for example, [0038]). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to incorporate the third precursor comprises calcium sulfate as such an addition would predictably allow for calcium replacement within the electrode material resulting in suppression of increases in battery thickness due to repeated charge / discharge cycles, and thus improving discharge capacity and thermal stability of the battery.
Claim(s) 1, 4, 8-9, and 11-14 is/are rejected under 35 U.S.C. 103 as being unpatentable over Gong et al (CN 110044989; citations directed to machine translation provided herein; hereafter Gong) in view of Oladeji.
Claim 1: Gong teaches a method of forming a lithium salt film (such as sensing electrode layer, further of a metal sulfate) (See, for example, [0023], [0053-55], [0093]).
Gong further teaches application of film via screen printing from a slurry mixture comprising binders and dispersants and subsequent sintering, such as at 700-1400C or 500-600C (See, for example, [0023], [0025]). Although such a temperature is not explicitly 100-800C, it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a temperature within the claimed range since in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art” a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191USPQ 90 (CCPA 1976).
Gong further teaches wherein the mixture comprises
a first and second precursor comprising a lithium ion (such as lithium sulfate) and an anion (such as sulphate) (see, for example , [0017], [0023], [0053-55], wherein a portion of the lithium sulfate could be interpreted as the first precursor and a portion as the second, alternatively it has taught mixture of sulfates, thus lithium metal sulfate could be interpreted as the first and a second metal sulfate as the second).
And a solvent (such as fluid medium for disclosed slurry ) (See, for example, [0023], [0025]).
And wherein: the lithium salt film comprises the lithium ion and the anion (such as LiSO4) (See, for example, [0017], [0023], [0053-55] [0093]);
Gong does not teach the remaining claimed steps of spraying the mixture while heating, and is silent as to the sensing electrode thickness.
Oladeji teaches a method for making a lithium salt electrode film (cathode material film, such as LiMPO4), (See, for example, abstract, [0060-0061], [0082])
Oladeji further teaches conventional slurry deposition methods for deposition of electrodes result in a variety of drawbacks making application cumbersome (See, for example, [0005-0011]). Oladeji has thus demonstrated that a method involving heating a substrate (see, for example, [0023], [0030], [0037], examples) and while heating, spraying a mixture of coating precursors onto the substrate to form a precursor film allows for improved electrode manufacturing and enhanced properties (See, for example, [0023], [0030], [0037] examples). The mixture of Oladeji further comprising: a first precursor comprising a lithium ion (such as lithium salt of acetate, sulfate, chloride, citrate, or nitrate) (See, for example, [0062]); a second precursor comprising an anion (such as various acids, metal salts, ammonia, phosphoric acid, sulfuric acid, etc) (see, for example, [0062], and a solvent (such as water) (see, for example, [0060]); And Oladeji teaches annealing the precursor film to form the lithium salt film having a thickness of about 2 micron (see, for example, [0066] ~1 micron / min for 2 minutes, or [0068]), or 10 micron (see, for example, [0072], [00777], wherein deposition proceeds at ~1 micron / minute at 10 minutes). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated the electrode deposition method of Oladeji including spraying onto a heated substrate to deposit the precursor film as such a method would overcome deficiencies of convention slurry coating, and provide enhance properties and manufacturability.
Claim 4: Oladeji further teaches wherein the solvent comprises water, or alcohol (methanol, ethanol, methoxypropanol) (see, for example, [0060], [0062] examples).
Claim 8: Gong further teaches wherein its film comprises at least one of lithium sulphate such (See, for example, [0061], [0083].
Claim 9: Gong further teaches wherein the substrate is a solid substrate comprising at least one of a metal, a metal oxide, a metal alloy, carbon, silicon (see, for example, Figures, [0020-0028] other deposited components of sensor such as YSZ, reference electrode, sealing layer, current collector)
Claim 11-13: Gong further teaches wherein: the mixture further comprises a third precursor comprising a second metal ion (such Calcium, Barium, or sodium) and the lithium salt film further comprises the second metal ion (such as LiSO4-CaSO4) (see, for example, [0017], [0053]).
Claim 14. Gong further teaches wherein sulfate precursors comprises mixture of lithium and calcium sulfate, thus inclusive of essentially >0 to < 100% of one relative to other (see, for example, [0017], [0053]). Although such a range is not explicitly wherein the lithium sulfate and the calcium sulfate are in a mole ratio of about one to one, it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a mole ratio within the claimed range since in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art” a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191USPQ 90 (CCPA 1976) and / or since generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical.(MPEP 2144.05 II A), and or since “[W]here the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation.” In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955).
Claim(s) 11-14 is/are alternatively rejected under 35 U.S.C. 103 as being unpatentable over Gong in view of Oladeji as applied to claim 1 above and further in view of Yan et al (“Solid State Sensor for Sulfur-Oxides Based on Stabilized Zirconia and Metal Sulphate” Chemistry Letters, pp635-638, 1992; hereafter Yan).
Claim 11-14: Gong in view of Oladeji teach the method of claims 1 and 11, but they do not explicitly teach an exemplary embodiment wherein the precursors and electrode comprise Lithium sulfate and Calcium sulfate, further at molar ratio of one to one. Yan teaches a method of preparing metal sulfate electrode films for SOx sensing (See, for example, abstract). Yan further teaches binary systems of lithium – calcium sulfate provide improved sensing characteristics including improved rate of recovery (See, for example, pg 637-638, Fig 4). Yan further teaches wherein the properties could be further tailored by adjusting the relative molar ratio of lithium sulfate to calcium sulfate (see, for example, pg 637-638, Fig 4; demonstrating a shift towards improved recovery response by moving from a molar ratio of 8:2 to 6:4). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a binary lithium sulfate- calcium sulfate precursor mixture and ultimate film since such a binary system provides enhanced sensing characteristics over lithium sulfate alone. Further although the disclosed molar ratios of 8:2 and 6:4 are not explicitly 1:1 as claimed, it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated such a molar ratio since the prior art has established that the relative mole ratio influences the resulting sensing properties and as the trend of sensing property improvement by decreasing the amount of lithium sulfate to calcium sulfate from 8:2 to 6:4 would appear to suggest that further decreases in the ratio may further lead to further improvements in sensing properties; and since discovery of an optimum value of a result effective variable in a known process is ordinarily within the skill of the art. In re Boesch, 617 F.2d 272, 276 (CCPA 1980), and since generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. (MPEP 2144.05 II A).
Claim(s) 16 is/are rejected under 35 U.S.C. 103 as being unpatentable over Oladeji in view of Marine Reynaud (“Design of new sulfate-based positive electrode materials for Li- and Na-ion batteries.” Material chemistry. Université de Picardie Jules Verne, 2013 PHD Dissertation; hereafter Raynaud) and Barker.
Claim 16: Oladeji teaches a method for making a lithium salt film (cathode material film, such as LiMPO4), (See, for example, abstract, [0060-0061], [0082]) the method comprising:
spraying a mixture onto a substrate having a temperature of between about 100 and 400 to form a precursor film (See, for example, [0023], [0030], [0037]). Although such a temperature is not about 180° C. to 220° C, it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have incorporated a temperature within the claimed range since in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art” a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191USPQ 90 (CCPA 1976).
the mixture comprising:
lithium acetate (See, for example, [0062]);
water (see, for example, [0060]);
and annealing the precursor film to form the lithium salt film having a thickness of about 2 micron (see, for example, [0066] ~1 micron / min for 2 minutes, or [0068]), or 10 micron (see, for example, [0072], [00777], wherein deposition proceeds at ~1 micron / minute at 10 minutes);
wherein: the lithium salt film comprises the lithium ion and the anion (such as LiMPO4) (See, for example, [0061], or [0082]);
and while annealing, the precursor film has a temperature of 400° C or 700° C (See, for example, [0066], [0073], [0078]).
Oladeji does not explicitly teach wherein the lithium salt film is a lithium sulfate film. Raynaud teaches a method of preparing positive electrode materials for Li-ion batteries (See, for example, abstract). Raynaud further teaches wherein replacing phosphate PO4 in LiMPO4 with sulfate SO4 results in attractive electrochemical properties, high-operating voltages, and adjustable polymorphism (See, for example abstract, pg 112-113, and 151-153). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to have replaced the phosphate with sulfate and made a lithium sulfate film since it would allow for attractive electrochemical properties, high-operating voltages and adjustable polymorphism.
Oladeji further teaches wherein the precursor can comprise sulfate ions (sulfuric acid) and ammonia (See, for example, [0062]), but is silent as to an appropriate precursor for forming a lithium sulfate film, so it does not explicitly teach wherein the mixture comprises ammonium sulfate. Barker similarly teaches a method of forming lithium battery electrode material, further of LiMPO4 typing (See, for example, [0006]). Barker further teaches it is known to replace phosphorus with sulfur in such structures, and such replacement is performed via using ammonium sulfate in the starting materials (see, for example, [0016]). Therefore it would have been obvious to one of ordinary skill in the art at the time before the effective filing date of the claimed invention to the second precursor comprise ammonium sulfate as such an addition would predictably allow for sulfur replacement of the phosphorus within the LiMPO4 electrode material film to produce the desired sulfate film, and since when a primary reference is silent as to a certain detail, one of ordinary skill would be motivated to consult a secondary reference which satisfies the deficiencies of the primary reference.
Conclusion
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/NATHAN H EMPIE/ Primary Examiner, Art Unit 1712