DETAILED ACTION
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 .
Response to Amendment
The examiner acknowledges the amendments as filed 12/22/2025. The amendments overcome the 102(a)(1) rejection as previously set forth in non-final rejection filed 09/22/2025, new grounds of rejection are outlined below.
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.
Claims 1-5, 15-17, and 19-20 are rejected under 35 U.S.C. 103 as being unpatentable over by (US-20200161706-A1) hereinafter referred to as ‘Cao’ in view of ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’
Regarding Claim 1,
Cao teaches a battery cell, comprising an anode, a cathode (Cao, “The Li∥NMC811 cells were prepared with 1.5 mAh cm−2 NMC811 and a 50 μm Li anode,”, see [0254]), a nonflammable electrolyte (Cao, “In some embodiments, an LSE comprises (i) an active salt; (ii) a solvent comprising an ether, a carbonate, a sulfone, an ester, a lactone, a sulfoxide, water, a flame retardant compound”, see [0005]), a separator configured to separate the anode and the cathode and permit lithium ion permeability there-through (Cao, “In some embodiments, a rechargeable battery comprises an LSE as disclosed herein, a cathode, an anode, and optionally a separator.”, see [0170]), and a solid-electrolyte interphase (SEI) layer on the surface of the anode or the cathode (Cao, “A reduced presence of free, unassociated solvent molecules increases coulombic efficiency (CE) of a lithium metal anode, facilitates formation of a stabilized SEI layer”, see [0142]).
Cao does not teach that the nonflammable electrolyte comprises essentially of triethyl phosphate (TEP).
Matsuda teaches an electrolyte that essentially of triethyl phosphate (TEP) (Matsuda, “The present study demonstrated that when the triethylphosphate-based electrolyte contains lithium nitrate and triethylphosphate forms a solvated complex by coordinating with Li ions, the O2 evolution rate could reach almost 100 % of that of the ideal two-electron reaction (O2/e– = 0.5) during the most part of the charging process, with the total oxygen evolution yield exceeding 90 %.”, see Abstract).
Matsuda teaches that triethyl phosphate (TEP) demonstrates increased performance with only TEP in the electrolyte, and other solvents do not yield the same effects (Matsuda, “It also should be noted that such high oxygen evolution efficiency was not observed when employing the electrolyte in which TEP was replaced with tetraethylene glycol dimethyl ether (TEGDME) (Figure S2). This result clearly indicates that the superior oxidation resistance of the TEP solvent contributed to the enhanced oxygen generation efficiency. We also performed the liner sweep voltammogram to confirm the potential window of TEP-based electrolyte. As a result, the results revealed that the TEP-based electrolyte is stable even up to 4.2 V”, see Results and Discussion).
Cao and Matsuda are analogous as they are both of the same field of electrolytes for lithium metal batteries.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have simplified the electrolyte solution as taught in Cao to the solution as taught in Matsuda in order to limit the solution to electrolyte solvents which demonstrate a benefits to stability and cycling.
Regarding Claim 2,
Modified Cao teaches the battery cell is fire-resistant (Cao, “The LSEs can include fire retardant compounds, rendering them low flammable or non-flammable, thereby also improving the safety of alkali metal batteries, such as Li metal and Na metal batteries.”, see [0168]).
Regarding Claim 3,
Modified Cao teaches the battery cell of claim 1, wherein the anode comprises lithium (Cao, “Embodiments of the disclosed low flammability or non-flammable LSEs are useful in batteries (e.g., rechargeable batteries), sensors, and supercapacitors. Suitable batteries include, but are not limited to, lithium metal batteries”, see [0169]).
Regarding Claim 4,
Modified Cao teaches the battery cell of claim 1, wherein the cathode comprises LiFeP04 (LFP) (Cao,” Exemplary cathodes for lithium metal or lithium-ion batteries include, but are not limited to, Li-rich Li1+wNixMnyCozO2 (x+y+z+w=1, 0≤w≤0.25), LiNixMnyCozO2 (NMC, x+y+z=1), LiCoO2 (LCO), LiNi0.8Co0.15Al0.05 O2 (NCA), LiNi0.5Mn1.5O4 spinel, LiMn2O4 (LMO), LiFePO4 (LFP)”, see [0175]).
Regarding Claim 15,
Modified Cao teaches the battery cell of claim 1, wherein the SEI layer is stable (Cao, “electrolyte, facilitate formation of a stable SEI layer, reduce the flammability of the electrolyte, or any combination thereof.”, see [0162]).
Regarding Claim 16,
Modified Cao teaches The battery cell of claim 1, wherein the lithium stripping and plating is reversible (Cao, “beneficial for achieving a high CE for reversible Li deposition stripping”, see [0229]).
Regarding Claim 17,
Modified Cao teaches The battery cell of claim 1, wherein the battery cell has Coulombic Efficiency (CE) selected from the group consisting of 95%, 95.1%, 95.2%, 95.3%, 95.4%, 95.5%,95.6%,95.7%, 95.8%, 95.9%, 96%, 96.1%, 96.2%, 96.3%, 96.4%, 96.5%, 96.6%, 96.7%, 96.8%, 96.9%, 97%, 97.1%, 97.2%, 97.3%, 97.4%, 97.5%, 97.6%, 97.7%, 97.8%, 97.9%, 98%, 98.1%, 98.2%, 98.3%, 98.4%, 98.5%, 98.6%, 98.7%, 98.8%, 98.9%, 99%, 99.1%, 99.2%,99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8%, 99.9%, and 100% (Cao, “Embodiments of a battery include an electrolyte as disclosed herein, an anode, and a cathode. The battery may have a coulombic efficiency 95%. In some embodiments”, see [0009]).
Regarding Claim 19,
Modified Cao teaches The battery cell of claim 1, wherein the SEI layer enhances lithium stripping and plating (Cao, “In summary, certain embodiments of the disclosed LSEs are cost-effective, enable dendrite-free plating, provide high CE, and/or greatly enhance fast charging and/or stable cycling of batteries.”, see [0191])
Regarding Claim 20,
Modified Cao does not teach wherein the battery cell is capable of achieving at least 5,000 charging and discharging cycles with at least 70% capacity retention.
However, Cao teaches that 500 cycles with a retention of 99% for up to 500 cycles (Cao, “with CE greater than 99%. … 300-500 cycles”, see [0184])
Considering that the battery composition is the same and that the SEI would be stabilized by 500 cycles, it would have been obvious to one of ordinary skill in the art before the effective fling date of the claimed invention to have extended the cycling to 5000 cycles and to not expect a retention of less than 70% (see Obvious to Try MPEP 2143 (I)(E)).
Claim 6, 9, 10-12, 18, and 21 are rejected under 35 U.S.C. 103 as being unpatentable over (US-20200161706-A1) hereinafter referred to as ‘Cao’ in view of ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’, in view of ‘Revealing Mechanism of Li3PO4 Coating Suppressed Surface Oxygen Release for Commercial Ni-Rich Layered Cathodes’ hereinafter referred to as ‘Gan’
Regarding Claim 6,
Cao does not teach wherein the SEI layer comprises Li3PO4.
Gan teaches wherein the SEI layer comprises Li3PO4 (Gan, “Herein, we systematically studied the critical role of the LPO protective layer through combining atomic-scale microscopy and in/ex situ techniques.”, Introduction).
Gan teaches that this layer suppresses oxygen release and improve the intensity of metal oxide bonds (Gan, “These advanced techniques make it possible to deeply reveal the mechanism of LPO coating suppressed oxygen release. Moreover, this approach of systematical investigation into the role of LPO layer during cycling of the Ni-rich layer oxides can be extended to deeply study many other surface modification strategies.”, Introduction)
Cao and Gan are analogous as they both relate to the same field of battery materials.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the claimed invention in order to suppress oxygen release, improve bonds, and improve the conductivity.
Regarding Claim 9,
Modified Cao teaches the battery cell of claim 6, wherein the SEI layer is formed by exposing the battery cell to 02 (Gan, “NCM811@LPO was prepared through a solvent-free in situ strategy...The mixed powder was sintered at 180 °C for 5 h under air atmosphere.”, see Methods) (The examiner notes air contains oxygen).
Regarding Claim 10,
Modified Cao teaches the battery cell of claim 9, wherein the battery cell is purged with 02 (Gan, “NCM811@LPO was prepared through a solvent-free in situ strategy...The mixed powder was sintered at 180 °C for 5 h under air atmosphere.”, see Methods).
Regarding Claim 11,
Modified Cao the battery cell of claim 9, wherein the continuous exposure to 02 is not required(Gan, “NCM811@LPO was prepared through a solvent-free in situ strategy...The mixed powder was sintered at 180 °C for 5 h under air atmosphere.”, see Methods) (The examiner notes that the there is only one non-continuous exposure as quoted above).
Regarding Claim 18,
Modified Cao teaches the battery cell of claim 9, wherein the battery cell has higher Coulombic Efficiency (CE) than the corresponding battery cell without exposing to 02 (Gan, see fig 3)
Regarding Claim 21,
Modified Cao teaches the battery cell of claim 9, wherein the battery cell has higher number of charging and discharging cycles with at least 70% capacity retention than the corresponding battery cell without exposing to 02 (Gan, see Figure (3d)).
Claim 12 is rejected under 35 U.S.C. 103 as being unpatentable over (US-20200161706-A1) hereinafter referred to as ‘Cao’ in view of (US-20170294687-A1) in view of ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’, in view of ‘Revealing Mechanism of Li3PO4 Coating Suppressed Surface Oxygen Release for Commercial Ni-Rich Layered Cathodes’ hereinafter referred to as ‘Gan’, as evidenced by ‘Lithium Batteries and the Solid Electrolyte Interphase (SEI)—Progress and Outlook’ hereinafter referred to as ‘Adensui’.
Regarding Claim 12,
Modified Cao teaches the battery cell of claim 9, wherein the SEI layer is formed by electrochemical reduction reaction (the examiner notes that the SEI is formed on the anode due to reduction for most cells, as evidenced by Adenusi (Adenusi, ‘In 1999, Aurbach et al. illustrated the SEI formation processes commencing from electrolyte reduction on electrode surfaces, see Abstract)) .
Claim 7 is rejected under 35 U.S.C. 103 as being unpatentable over (US-20200161706-A1) hereinafter referred to as ‘Cao’ in view of ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’, in view of (US-20170294687-A1) hereinafter referred to as ‘Burshtain’
Regarding Claim 7,
Cao does not teach the battery cell of claim 1, wherein the SEI layer comprises poly-phosphate.
Burshtain teaches wherein the SEI layer comprises poly-phosphate (Burshtain, “examples for materials in buffering zone(s) 110B are ionic conductors which are medium electronic conductors, such as inorganic borates, phosphates or polyphosphates and organic polymers such as polypyrrole and polyaniline—the particle size of which and thickness of buffering zone(s)”, see [0057])
Burshtain teaches that this buffering zone consisting of polyphosphates allows for the prevention of dendrite growth on the anode (Burshtain, “Anodes and/or electrolytes have buffering zones for partly reducing and gradually introducing lithium ions into the anode for lithiation, to prevent lithium-ion accumulation at the anode electrolyte interface and consequent metallization and dendrite growth”, see [0041]).
Cao and Burshtain are analogous as they are both of the same field of anode materials.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the material as taught in Cao with a polyphosphate SEI as taught in Burshtain in order to prevent dendrite growth.
Claim 8 is rejected under 35 U.S.C. 103 as being unpatentable over (US-20200161706-A1) hereinafter referred to as ‘Cao’ in view of ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’ in view of ‘Revealing Mechanism of Li3PO4 Coating Suppressed Surface Oxygen Release for Commercial Ni-Rich Layered Cathodes’ hereinafter referred to as ‘Gan’ in view of (US-20170294687-A1) hereinafter referred to as ‘Burshtain’.
Regarding Claim 8,
Cao does not teach where the SEI comprises Li3PO4 and poly-phosphate.
Gan teaches wherein the SEI layer comprises Li3PO4 (Gan, “Herein, we systematically studied the critical role of the LPO protective layer through combining atomic-scale microscopy and in/ex situ techniques.”, Introduction).
Gan teaches that this layer suppresses oxygen release and improve the intensity of metal oxide bonds (Gan, “These advanced techniques make it possible to deeply reveal the mechanism of LPO coating suppressed oxygen release. Moreover, this approach of systematical investigation into the role of LPO layer during cycling of the Ni-rich layer oxides can be extended to deeply study many other surface modification strategies.”, Introduction)
Cao and Gan are analogous as they both relate to the same field of battery materials.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the claimed invention in order to suppress oxygen release, improve bonds, and improve the conductivity.
Burshtain teaches wherein the SEI layer comprises poly-phosphate (Burshtain, “examples for materials in buffering zone(s) 110B are ionic conductors which are medium electronic conductors, such as inorganic borates, phosphates or polyphosphates and organic polymers such as polypyrrole and polyaniline—the particle size of which and thickness of buffering zone(s)”, see [0057])
Burshtain teaches that this buffering zone consisting of polyphosphates allows for the prevention of dendrite growth on the anode (Burshtain, “Anodes and/or electrolytes have buffering zones for partly reducing and gradually introducing lithium ions into the anode for lithiation, to prevent lithium ion accumulation at the anode electrolyte interface and consequent metallization and dendrite growth”, see [0041]).
Cao and Burshtain are analogous as they are both of the same field of anode materials.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the material as taught in Cao with a polyphosphate SEI as taught in Burshtain in order to prevent dendrite growth.
Claim 13 is rejected under 35 U.S.C. 103 as being unpatentable over (US-20200161706-A1) hereinafter referred to as ‘Cao’ in view of ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’ in view of (US-20200321603-A1) hereinafter referred to as ‘Xiao’
Regarding Claim 13,
Cao does not teach the battery cell of claim 1, wherein the thickness of the SEI layer is in a range of about 0.05 um to about 50 um.
Xiao Teaches wherein the thickness of the SEI layer is in a range of about 0.05 μm to about 50 μm (Xiao, “the SEI layer 121 can have a thickness of about 200 nm to about 5 μm.”, see [0033]).
The examiner takes note of the fact that the prior art range of 200 nm to about 5 μm broadly overlaps the claimed range of 0.05 μm to about 50 μm. Absent any additional and more specific information in the prior art, a prima facie case of obviousness exists. In re Peterson, 315F.3d 1325, 1330, 65 USPQ2d 1379 (Fed. Cir. 2003). MPEP 2144.05.
Xiao teaches that when the SEI is thicker than the energy density decreases along with the ionic conductivity (Xiao, “As thickness T of the SEI layer(s) 121 increases, the ionic conductivity of the SEI layer(s) 121 and the volumetric energy density of the battery cell decreases,”, see [0033])
Cao and Xiao are analogous as they are both of the same field of battery materials.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the SEI as taught in Cao with the SEI thickness as taught in Xiao in order to minimize the reduction in ionic conductivity while maximizing the energy density.
Claim 14 is rejected under 35 U.S.C. 103 as being unpatentable over (US-20200161706-A1) hereinafter referred to as ‘Cao’ in view of ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’ in view of ‘Revealing Mechanism of Li3PO4 Coating Suppressed Surface Oxygen Release for Commercial Ni-Rich Layered Cathodes’ hereinafter referred to as ‘Gan’ in further view of ‘Li metal coated with amorphous Li3PO4 via magnetron sputtering for stable and long-cycle life lithium metal batteries’ hereinafter referred to as ‘Wang’
Regarding Claim 14,
Modified Cao does not teach wherein the SEI layer is formed during a battery cell charge cycle.
Wang teaches wherein the SEI layer is formed during a battery cell charge cycle (Wang, “To engender SEI enriched with LiF, Li2CO3 or Li3PO4 upon graphite electrodes, three prevalent electrolyte additives were employed: fluoroethylene carbonate (FEC), vinylene carbonate (VC), and lithium difluorophosphate (LiDFP), which are precursory to the formation of LiF, Li2CO3 and Li3PO4, respectively (Figure 1a and Figure S1)”, see Results and Discussion).
Wang teaches that Li3PO4 rich SEI demonstrated superior rate capacity (Wang, “Remarkably, when these graphite electrodes were assembled into full cell, the graphite electrode with Li3PO4-rich SEI showcase a superior rate capability, preserving over 60 % capacity even at 6 C charging rate (Figure S7).”, see Results and Discussion).
Cao and Wang are analogous as they are both of the same field of battery materials and SEI.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the electrolyte content as taught in Cao with that which is taught in Wang in order to allow for an SEI rich in Li3PO4 to form during cycling and allow for improve performance.
Response to Arguments
Applicant's arguments filed 12/22/2025 have been fully considered but they are not persuasive.
On pg. 7, the applicant argues:
“From the foregoing, it can be appreciated that, while the electrolyte composition of Cao can include a lithium salt and a flame-retardant solvent such as TEP, the electrolyte composition of Cao further requires a diluent, different from the solvent, in addition to the lithium salt and flame-retardant solvent. Accordingly, Cao fails to teach or suggest "a nonflammable electrolyte consisting essentially of a lithium salt and triethyl phosphate (TEP)" as recited in amended claim 1.”
This is convincing, as the electrolyte of Cao has many components in addition to the TEP. However, further search and consideration has found ‘Highly Efficient Oxygen Evolution Reaction in Rechargeable Lithium–Oxygen Batteries with Triethylphosphate-Based Electrolytes’ hereinafter referred to as ‘Matsuda’, which teaches the TEP as the only solvent along with a lithium salt (Matsuda, “Four TEP-based electrolytes were prepared with varying concentrations of lithium nitrate (LiNO3) and lithium bis(trifluoromethanesulfonyl)imide (LiTFSI), both of which are widely used in Li–O2 batteries. (2,16−19) They are designated as A (1 M LiNO3 in TEP), B (3 M LiNO3 in TEP), C (1 M LiTFSI in TEP), and D (1 M LiTFSI + 1 M LiNO3 in TEP).”, see Results and Discussion). As outlined above, Matsuda demonstrates that beneficial effects can be had when TEP is the only solvent used with lithium metal. This would make it obvious to one of ordinary skill in the art to have modified the electrolyte as taught in ‘Cao’ to be simplified to just the TEP. All similar arguments related to claims dependent on claim 1 remain rejected.
Conclusion
35. 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.
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/S.P.M./Examiner, Art Unit 1752
/NICHOLAS A SMITH/Supervisory Primary Examiner, Art Unit 1752