Prosecution Insights
Last updated: May 29, 2026
Application No. 18/710,382

Spray Pyrolysis of Li-Salt Films

Final Rejection §102§103
Filed
May 15, 2024
Priority
Nov 15, 2021 — nonprovisional of PCTUS2021059339
Examiner
EMPIE, NATHAN H
Art Unit
1712
Tech Center
1700 — Chemical & Materials Engineering
Assignee
Massachusetts Institute Of Technology
OA Round
2 (Final)
44%
Grant Probability
Moderate
3-4
OA Rounds
1y 7m
Est. Remaining
86%
With Interview

Examiner Intelligence

Grants 44% of resolved cases
44%
Career Allowance Rate
310 granted / 709 resolved
-21.3% vs TC avg
Strong +42% interview lift
Without
With
+42.5%
Interview Lift
resolved cases with interview
Typical timeline
3y 7m
Avg Prosecution
49 currently pending
Career history
759
Total Applications
across all art units

Statute-Specific Performance

§101
0.2%
-39.8% vs TC avg
§103
86.5%
+46.5% vs TC avg
§102
2.9%
-37.1% vs TC avg
§112
1.4%
-38.6% vs TC avg
Black line = Tech Center average estimate • Based on career data from 709 resolved cases

Office Action

§102 §103
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 . Applicant's submission filed on 3/11/26 has been entered. Claims 1-10, 16, and 21 are currently pending examination, claims 15 and 17 are withdrawn and claims 11-14, and 18-20 are canceled. 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 8-10 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 consisting of: at least one first precursor comprising a lithium ion (such as comprising lithium salt of acetate, sulfate, chloride, citrate, or nitrate and interpreted optionally as in combination with ligand(s)) (See, for example, [0062]); at least one second precursor comprising an anion (such as comprising various acids, metal salts, ammonia, phosphoric acid, etc and interpreted optionally as in combination with ligand(s)) (see, for example, [0062]); and at least one solvent (such as water and / or optionally further as ligand(s) such as urea or ammonia or others capable of acting as a solvent) (see, for example, [0060-62]); and annealing the precursor film to decompose the precursor film thereby causing the anion to react with the lithium ion to form the lithium salt film (such as formation of LiMPO4 film from li ion and PO4 anion) having a thickness of about 2 micron (see, for example, [0061], [0066], [0082], ~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]). As presently claimed, the open "comprising" language in the limitations directed to components of "at least one first / second precursor" allows interpretation of these precursors as being inclusive of any combination or mixture of further species (such as inclusive of ligands, etc) as long as the first / second precursor respectively contains "a lithium ion" / "anion" therein. 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 at least one solvent comprises water, or alcohol (methanol, ethanol, methoxypropanol) (see, for example, [0060], [0062] examples). Claim 5: Oladeji further teaches wherein the at least one first precursor comprises at least one of lithium acetate, or lithium nitrate (see, for example, [0062], examples). Claim 6: Oladeji further teaches wherein the at least one 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 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 at least one 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 at least one 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 at least one 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 have the at least one 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) 1, 4, and 8-9 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 consisting of: at least a first precursor comprising a lithium ion (such as comprising lithium salt of acetate, sulfate, chloride, citrate, or nitrate and interpreted optionally as in combination with ligand(s)) (See, for example, [0062]);at least a second precursor comprising an anion (such as comprising various acids, metal salts, ammonia, phosphoric acid, etc and interpreted optionally as in combination with ligand(s)) (see, for example, [0062]); and at least one solvent (such as water or optionally further as ligand(s) such as urea or ammonia or others capable of acting as a solvent) (see, for example, [0060-62]). Oladeji further teaches annealing the precursor film, wherein film has a temperature of 400° C or 700° C during annealing to decompose the precursor film thereby causing the anion to react with the lithium ion to form the lithium salt film having a thickness of about 2 micron (see, for example, [0061], [0066], [0073], [0078] ,[0082], ~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); 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 enhanced properties and manufacturability. As presently claimed, the open "comprising" language in the limitations directed to components of "at least one first / second precursor" allows interpretation of these precursors as being inclusive of any combination or mixture of further species (such as inclusive of ligands, etc) as long as the first / second precursor respectively contains "a lithium ion" / "anion" therein. Claim 4: Oladeji further teaches wherein the at least one 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(s) 16 and 21 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 consisting of: at least one first precursor comprising lithium acetate (and interpreted optionally as in combination with ligand(s)) (See, for example, [0062]); at least one second precursor comprising an anion (such as comprising various acids, metal salts, ammonia, phosphoric acid, etc and interpreted optionally as in combination with ligand(s)) (see, for example, [0062]); at least one solvent (such as water or optionally further as ligand(s) such as urea or ammonia or others capable of acting as a solvent) (see, for example, [0060-62]); and annealing the precursor film to decompose the precursor film thereby causing the anion to react with the lithium ion to form the lithium salt film (such as formation of LiMPO4 film from li ion and PO4 anion) having a thickness of about 2 micron (see, for example, [0061], [0066], [0082], ~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]). 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 within the at least one second precursor 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 at least one second 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. As presently claimed, the open "comprising" language in the limitations directed to components of "at least one first / second precursor" allows interpretation of these precursors as being inclusive of any combination or mixture of further species (such as inclusive of ligands, etc) as long as the first / second precursor respectively comprises "lithium sulfate" / "ammonium sulfate" therein. Claim 21: Oladeji has taught wherein the at least one solvent comprises water (See, for example, [0060-62]). Response to Arguments Applicant's arguments filed 3/11/26 have been fully considered but they are not persuasive. In response to applicant's argument that the references fail to show certain features of the invention, it is noted that the features upon which applicant relies (i.e., “the mixture of claim 1 (and 16) does not include a ligand”) are not recited in the rejected claim(s). Although the claims are interpreted in light of the specification, limitations from the specification are not read into the claims. See In re Van Geuns, 988 F.2d 1181, 26 USPQ2d 1057 (Fed. Cir. 1993). Even through Applicant amended to “the mixture consisting of” the retention / addition of open "comprising" language within the limitations of the particular components of the mixture in claims 1/16 results in "at least one first precursor comprising" and "at least one second precursor comprising" as being inclusive of any combination or mixture of materials as long as the first / second precursor respectively contains "a lithium ion" / "anion". Thus, for example, the “at least first precursor” could be interpreted as the combination of lithium salt and the argued ligand(s). By such an interpretation “the at least first precursor” still comprises a “lithium ion” and this ion is present and reacts with the anion to form the lithium salt film. Alternatively as noted in the rejections above the present phrasing of “at least one solvent” is additionally open to include water and the argued ligand(s) such as urea or ammonia or other ligands capable of acting as a solvent to any particular solute. As such, the present claim phrasing does not effectively exclude the presence of the argued ligand(s). Applicant’s arguments directed to claim 17 is moot as claim 17 is not presently pending examination as it was withdrawn from consideration for being drawn to a nonelected invention (see 10/20/25 Applicant’s Response to requirement for unity of invention and the 12/11/25 Non-Final Office action). As to the remaining dependent claims they remain rejected as no additional separate arguments are provided. 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 NATHAN H EMPIE whose telephone number is (571)270-1886. The examiner can normally be reached Monday-Thursday 5:30AM - 4 PM. Examiner interviews are available via telephone, in-person, and video conferencing using a USPTO supplied web-based collaboration tool. To schedule an interview, applicant is encouraged to use the USPTO Automated Interview Request (AIR) at http://www.uspto.gov/interviewpractice. If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Michael Cleveland can be reached at 571-272-1418. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300. Information regarding the status of published or unpublished applications may be obtained from Patent Center. Unpublished application information in Patent Center is available to registered users. To file and manage patent submissions in Patent Center, visit: https://patentcenter.uspto.gov. Visit https://www.uspto.gov/patents/apply/patent-center for more information about Patent Center and https://www.uspto.gov/patents/docx for information about filing in DOCX format. For additional questions, contact the Electronic Business Center (EBC) at 866-217-9197 (toll-free). If you would like assistance from a USPTO Customer Service Representative, call 800-786-9199 (IN USA OR CANADA) or 571-272-1000. /NATHAN H EMPIE/Primary Examiner, Art Unit 1712
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Prosecution Timeline

May 15, 2024
Application Filed
Dec 11, 2025
Non-Final Rejection mailed — §102, §103
Feb 13, 2026
Interview Requested
Feb 20, 2026
Applicant Interview (Telephonic)
Feb 20, 2026
Examiner Interview Summary
Mar 11, 2026
Response Filed
Apr 14, 2026
Final Rejection mailed — §102, §103 (current)

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