DETAILED ACTION
Notice of Pre-AIA or AIA Status
1. The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Information Disclosure Statement
2. This is an acknowledgment of the applicant’s IDS filed 03 November 2025, which was considered by the examiner.
Response to Amendment
3. The applicant’s response dated 05 November 2025 has been entered into the record and is considered fully responsive. The applicant’s amendment do not add any new matter and have support for the new elemental ratio as supported by the two inventive examples (¶69 and ¶75). Currently, Claims 1, 2, 3, 4, and 5 are pending and under examination.
Claim Rejections - 35 USC § 103
4. 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.
5. The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
6. Claim 1 is rejected under 35 U.S.C. 103 as being unpatentable over Zhu et al. and Gupta et al., and Browne et al.
Zhu et al. (“Layered Fe-Substituted LiNiO2 Electrocatalysts for High-Efficiency Oxygen Evolution Reaction,” ACS Energy Lett. 2017, 2, 1654−1660 – previously presented) is directed toward an OER-catalyst with iron-doping (pg. 1654: title and abstract). Gupta et al. (“High-Rate Oxygen Evolution Reaction on Al-Doped LiNiO2,” Adv. Mater. 2015, 27, 6063-6067 – previously presented) is drawn toward an OER-catalyst (pg. 6063: title and abstract). Browne et al. (Determining the importance of the electrode support and fabrication method during the initial screening process of an active catalyst for the oxygen evolution reaction,” J. Mater. Chem. A 2018, 6, 14162-14169 – previously presented) is a study evaluating electrode supports for OER (pg. 14162: title and abstract).
Regarding Claim 1, Zhu et al. discloses an iron-doped lithium nickel oxide catalyst for use as an OER catalyst (pg. 1654: title and abstract) which is deposited onto a glassy carbon electrode (i.e.: a conductive support) for electrochemical testing (Supporting information on pg. 4-5: 4. Electrochemical characterization). Zhu et al. indicates that doping LiNiO2 with iron to form a catalyst layer with the formula Li1Ni0.8Fe0.2O2 makes a layered structure (i.e.: rock salt structure) and improved OER performance (pg. 1655). The present application (cited as US Pub. No. 2023/0279566 A1) indicates that a rock salt type structure is layered as per FIG. 4 and ¶51. Zhu et al. indicates that the improvement in OER performance is a result of the interaction between Li, Ni, and Fe in the materials and the layered structure is used to stabilize the high valence states of Ni and Fe (pg. 1659). However, Zhu et al. does not disclose further doping of the catalyst layer with aluminum ions.
Gupta et al. discloses doping lithium nickel oxide with aluminum (pg. 6063: title and abstract). On page. 6063, Gupta indicates that using a combustion synthesis method, the maximum doping with aluminum to form a pure material is less than 40% (based on 2 mol of oxygen). Moreover, Gupta et al. indicates the two variants of Al-doped LiNiO2 synthesized using the combustion method (Li1Ni0.9Al0.1O2 and Li1Ni0.8Al0.2O2) allow nickel to maintain a high oxidation state (Ni3+) during the synthesis resulting in better ordering of Li1+ and Ni3+ in their layers (pg. 6063-4). In fact, Li1Ni0.8Al0.2O2 resulted in improved OER performance showing higher current densities at higher overpotentials which were comparable to the benchmark IrO2 catalyst (Gupta et al. on pg. 6065-6). On pg. 6067, Gupta et al. also teaches that Li1Ni0.8Al0.2O2 exhibits long term stability in alkaline solutions. Therefore, Gupta et al. indicates that doping with Al improves the OER activity of lithium nickel oxides.
The combination of Zhu et al. and Gupta et al. disclose the electrode substrate as glassy carbon, but does not disclose the use of nickel or a nickel alloy as an electrode support. Browne et al.is a study aimed at selecting an electrode support for screening new OER catalysts (pg. 14162). Browne et al. indicated that the ideal support for new catalyst screening is electrically conductive, corrosion resistant, and electrochemically inert in alkaline electrolytes (pg. 14164). Browne et al. specifically tested the OER performance of a catalytic RuO2 layer deposited onto Pt, Ti, Ni, and glassy carbon substrates of different geometries (pg. 14163: Introduction). Browne et al. found that Ti and Pt discs meet all of the standards for the ideal support described above (pg. 14168: conclusion). Moreover, Browne et al. discloses that RuO2 on glassy carbon electrode has inferior OER activity and further loses activity as the current density increases indicating that it is not an ideal substrate for an OER catalyst. Browne et al. further indicates that bare nickel foam, though not an ideal substrate for catalyst screening, with its large surface area has significant catalytic activity for OER (pg. 14166: Electrochemical characterization: cyclic voltammetry/inherent electrochemistry). Using a nickel foam substrate would likely increase the OER activity of any catalyst deposited on top it. Therefore, a catalyst layer (e.g.: Al and Fe-doped lithium nickel oxide) deposited onto Ni-foam as the electrode substrate would results in higher OER activity when compared to the same catalyst deposited onto a glassy carbon electrode.
It would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention to prepare an aluminum-doped Li1Ni0.8Fe0.2O2 anode catalyst for the oxygen evolution reaction using the combustion method disclosed by the combination of Zhu et al. and Gupta et al. targeting lower levels of aluminum and iron (less than 0.2 mol per 2 moles O) on a nickel foam support as taught by Browne et al. The stoichiometry of aluminum is a result-effective variable, i.e., a variable which achieves a recognized result, and the determination of the optimum or workable ranges of said variable might be characterized as routine experimentation (See MPEP 2144.0.II.B.). Accordingly, it would have been obvious to one of ordinary skill in the art before the effective filing date of the invention to have discovered the optimum or workable ranges of the elemental levels of lithium, nickel, iron, aluminum and oxygen including values within the claimed range, through routine experimentation by varying the level of aluminum precursors used in the synthesis of the anode material. One would have been motivated to do so in order to form an anode catalyst doped with aluminum to form a material with enhanced OER activity.
7. Claim 2 is rejected under 35 U.S.C. 103 as being unpatentable over Zhu et al., Gupta et al., and Browne et al. as applied to Claim 1 above and further in view of Belharouak et al.
Belharouak et al. (US Pub. No. 2020/0235390 A1 – previously presented) is directed toward a lithium composite oxide comprising nickel, iron, and aluminum (title and abstract).
Regarding in Claim 2, the combination of Zhu et al., Gupta et al., and Browne et al. disclose the anode material as per Claim 1 above, but only provides XRF peak intensity data for Fe-doped LiNiO2 (Zhu et al.: Figure 4 on page 1657) and Al-doped LiNiO2 (Gupta et al.: Figure 1 on pg. 6064). A lithium composite oxide comprising nickel, iron, and aluminum prepared as per the combustion method, that is calcining in oxygen, (regardless of the end use of the material) would have a unique XRF pattern, from which the intensities of the diffraction peaks of the (003) plane and the (104) plane could be derived. Belharouak et al. discloses a lithium metal oxide in two different embodiments ¶18-20, with the first embodiment having a range of compositions for Li1+wNixFeyAlzO2 and the second embodiment with a more specific formula of Li1Ni0.8Fe0.1Al0.1O2 which are prepared in a manner similar to the combustion method of Gupta et al. (Belharouak et al. ¶32-34). Both of Belharouak’s embodiments overlap with the limitations of the stoichiometry of the catalyst layer disclosed in Claim 1. Belharouak et al. indicates that XRD can be used to understand the extent of cation mixing pertaining to Ni2+ and Li1+ ions in particular the ratio of the peak intensities of the (003) and (104) as discussed in ¶39 and shows in FIG. 2. Belharouak et al. discloses the ratio of the (003) to (104) for all prepared lithium transition metal oxides was greater than 1.5. With respect to Belharouak’s second embodiment, a prima facie case of obviousness exists as an example from the prior art falls within the claimed range. See MPEP 2144.05(I) - OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
8. Claim 3 is rejected under 35 U.S.C. 103 as being unpatentable over Zhu et al., Gupta et al., and Browne et al. as applied to Claim 1 above and further in view of Mitsushima et al.
Mitsushima et al. (US Pub. No.2020/0407860 A1 – previously presented) is directed at an electrode for electrolysis and a method of manufacturing one (title and abstract).
Regarding Claim 3, the combination of Zhu et al., Gupta et al., and Browne et al. disclose the anode catalyst material on a nickel-based substrate as per Claim 1 above, but does not disclose an intermediate layer disposed between the conductive substrate and the catalyst layer.
Mitsushima et al. discloses an electrode for electrolysis comprising a nickel-based substrate with an intermediate layer with a composition of LixNi2-xO2 (0.02≤x≤0.5), and a catalyst layer (abstract; ¶22, 26, 51, 60, 68; Claims 1 and 4). Mitsushima et al. further teaches that the intermediate layer suppresses corrosion or degradation of the electrically conductive substrate and firmly fixes the catalyst layer to the electrically conductive substrate, and facilitates electric current conduction to the catalyst layer ¶50-51. Additionally, Mitsushima et al. teaches the catalyst layer may be an anode material to promote the OER (¶55-57). Therefore, it would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention to modify the alkaline water electrolysis anode as per Zhu et al., Gupta et al., and Browne et al. by inserting Mitsushima’s intermediate layer between the nickel substrate and the Al and Fe-doped LiNiO2 catalyst layer with the reasonable expectation of forming an alkaline water electrolysis anode with improved cohesion and electrical conductivity (facilitated by the intermediate layer) as indicated by Mitsushima et al. (¶55-57).
9. Claims 4 and 5 are rejected under 35 U.S.C. 103 as being unpatentable over Belharouak et al. in view of Zhu et al., Gupta et al., and Mitsushima et al.
Regarding Claim 4, Belharouak et al. discloses the method of preparing a lithium composite oxide with the general formula (Li1NixFeyAlzO2, where 0<x<1; 0<y≤0.2; 0<z≤0.2, and x+y+z=1) and a specific example of Li1Ni0.8Fe0.1Al0.1O2 (¶20 and Claim 3) with a layered structure (i.e.: rock salt type). The present application (cited as US Pub. No. 2023/0279566 A1) indicates that a rock salt type structure is layered as per FIG. 4 and ¶51. The method of Belharouak et al. is explained in ¶32-34. The first step is to prepare an aqueous solution of lithium, nickel, iron, and aluminum in the presence of citric acid and forming a gel out of said solution (¶32). The gel is then heat treated to form a precursor powder and calcining in the presence of oxygen from 600 to 900℃ to form the lithium metal oxide (¶33). It has been held that a prima facie case of obviousness exists when the prior art discloses an example that is contained in or overlaps the claimed range (i.e.: the second embodiment of Belharouak et al. is similar to or approaching the elemental composition of Claim 4 and the calcining temperature range of Belharouak et al. overlaps with the temperature range of Claim 4). See MPEP 2144.05(I) - OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
However, Belharouak et al. is silent on the OER activity of Li1NixFeyAlzO2 (e.g.: Li1Ni0.8Fe0.1Al0.1O2). Zhu et al. and Gupta et al. disclose the effect on the oxygen evolution reaction activity of doping LiNiO2 with iron and aluminum, respectively,
Zhu et al. discloses an iron-doped lithium nickel oxide catalyst for use as an OER catalyst (pg. 1654: title and abstract) indicating that a catalyst layer comprising Fe-doped LiNiO2 makes a layered structure (i.e.: rock salt structure) with improved OER performance (pg. 1655). Zhu et al. indicates that the improvement in OER performance is a result of the interaction between Li, Ni, and Fe in the materials and the layered structure is used to stabilize the high valence states of Ni and Fe (pg. 1659).
Gupta et al. discloses doping lithium nickel oxide with aluminum (pg. 6063: title and abstract). On page. 6063, Gupta indicates that using a combustion synthesis method, the maximum doping with aluminum to form a pure material is less than 40% (based on 2 mol of oxygen). Moreover, Gupta et al. indicates the two variants of Al-doped LiNiO2 synthesized using the combustion method (Li1Ni0.9Al0.1O2 and Li1Ni0.8Al0.2O2) allow nickel to maintain a high oxidation state (Ni3+) during the synthesis resulting in better ordering of Li1+ and Ni3+ in their layers (pg. 6063-4). In fact, Li1Ni0.8Al0.2O2 resulted in improved OER performance showing higher current densities at higher overpotentials which were comparable to the benchmark IrO2 catalyst (Gupta et al. on pg. 6065-6). On pg. 6067, Gupta et al. also teaches that Li1Ni0.8Al0.2O2 exhibits long term stability in alkaline solutions. Therefore, Gupta et al. indicates that doping with Al improves the OER activity of lithium nickel oxides.
It would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention to use the lithium metal oxide taught by Belharouak et al. as an alkaline water electrolysis anode given the teachings of Zhu et al. and Gupta et al. with the reasonable expectation of forming an effective OER anode catalyst since Al and Fe-doping are both known to improve OER activity in alkaline aqueous electrolytes.
Belharouak et al. in view of Zhu et al. and Gupta et al. does not disclose applying the metal ion solution to the electrically conductive substrate prior to formation of the lithium metal oxide via calcination. Mitsushima et al. discloses forming a lithium-nickel oxide layer by preparing an aqueous solution of said elements (or cations), applying the solution to the nickel or nickel alloy substrate (i.e.: electrically conductive substrate), and subsequently heat treating the substrate (¶68). According to ¶69 of Mitsushima et al., the temperature of the heat treatment step ranges from about 450 to 600 ℃ and the calcination takes place in air (i.e.: an oxygen-containing atmosphere ¶92). The lithium-nickel oxide layer of Mitsushima et al. provides strong adhesion to the conductive substrate and allows facile electron transfer from the substrate (¶55-57). It would be obvious to one of ordinary skill in the art to modify the method of Belharouak et al. (in view of Zhu et al. and Gupta et al.) by applying the ion-containing solution to Mitsushima’s nickel substrate prior to heat treatment with the reasonable expectation of preparing a layered Li1NixFeyAlzO2 catalyst with strong adhesion onto a nickel substrate resulting in effective OER catalyst for alkaline water hydrolysis.
Regarding Claim 5, Belharouak et al, in view of Zhu et al, Gupta et al, and Mitsushima et al. discloses the method for producing an alkaline water electrolysis anode according to Claim 4. Belharouak et al. discloses the thermal treatment step of the aqueous or gelled material in the presence of oxygen (¶33) and Mitsushima et al. discloses Mitsushima et al. discloses coating the electrically conductive substrate with the precursor solution to coat the electrically conductive substrate (¶68-69). Neither reference supplies the exact partial pressure of oxygen used during the calcining step. The synthesis method discloses in Zhu et al. uses a high temperature calcining step (i.e.: 850 ℃) under a pure oxygen atmosphere (1 atm) to form layered LiNi0.8Fe0.2O2 as opposed to the cubic form of the same material (Supporting Information pg. 1: Experimental Section – 1. Synthesis). The former species is reported to have the higher OER activity (Zhu et al. on pg. 1659). It would have been obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention to set the partial pressure of oxygen to 1 atm when preparing the anode catalyst as per the combination of Belharouak et al, in view of Zhu et al, Gupta et al, and Mitsushima et al. with the reasonable expectation of forming the more catalytically active crystal structure (i.e.: layered vs. cubic) of Li1NixFeyAlzO2 (e.g.: Li1Ni0.8Fe0.1Al0.1O2).
Response to Arguments
10. Applicant's arguments filed 05 November 2025 have been fully considered but they are not persuasive as explained below.
11. As indicated in the first Office Action dated 14 July 2025, the closest prior art pertaining to independent Claim 1 is the combination of Zhu et al. and Gupta et al. even with the narrowed elemental ranges of amended Claim 1. As previously explained, Zhu et al. discloses an iron-doped lithium nickel oxide catalyst for use as an OER catalyst (pg. 1654: title and abstract) using a series of different levels of iron-doping. The electrochemical data is compared on pg. 1656 in Fig. 3a, Fig. 3b, Fig. 3e, and Fig. 3f. The general formula for the Fe-doped materials is: Li1Ni1-xFexO2 where x is the levels of doping (e.g.: x =0.1, 0.2, or 0.3). The best electrochemical performance was found when x=0.2 as that anode material has the lowest overpotential for OER (Fig. 3a), the highest OER current at a given potential (Fig. 3b), the lowest Tafel slope (Fig. 3e), and the lowest electrical impedance (Fig. 3f). When x=0.3, the resultant electrochemical performance was significantly worse. This change in performance suggests that the iron level in an OER catalyst should at most be 0.2 (which aligns with the claimed range of amended Claim 1) as per pg. 1656 in Fig. 3a, Fig. 3b, Fig. 3e, and Fig. 3f. Zhu et al. indicates that the improvement in OER performance is a result of the interaction between Li, Ni, and Fe in the materials and the layered structure is used to stabilize the high valence states of Ni and Fe (pg. 1659). Zhu et al. fails to disclose doping of LiNiO2 with elements other than Fe.
To address that deficiency in light of the limitations of (amended) Claim 1, the examiner modified Zhu et al. with Gupta et al. The latter discloses doping lithium nickel oxide with aluminum (pg. 6063: title and abstract). On page. 6063, Gupta et al. indicates that using a combustion synthesis method, the maximum doping with aluminum to form a pure material is less than 40% (based on 2 mol of oxygen). Doping with aluminum is hypothesized to allow nickel to maintain a high oxidation state (Ni3+) during the synthesis resulting in better ordering of Li1+ and Ni3+ in their layers (pg. 6063-4). The doping ratios (Ni to Al) synthesized by Gupta et al. included: (a) 0.65 Ni to 0.35 Al; (b) 0.70 Ni to 0.30 Al; (c) 0.75 Ni to 0.25 Al; (d) 0.80 Ni to 0.20 Al; and (e) 0.90 Ni to 0.10 Al. When comparing the current density of the OER reaction at 1.7 V RHE, the worst performing composition by at least 120 mA/mg oxide has the ratio of 0.65 Ni to 0.35 Al (supporting information pg. 10: Figure S3). The other ratios showed a current density of at least 250 mA/mg oxide which suggests that lowering the level of Al (below 0.35) is beneficial to electrochemical performance.
Therefore, combining the teachings above would suggest that the incorporation of both Al and Fe at a level less than 0.2 relative to Ni in a doped-LiNiO2 OER material will result in improved electrochemical performance. The applicant has provided data (¶69 and ¶75 cited as US Pub. No. 2020/0235390 A1) supporting the narrowed range of amended Claim 1. However, the data provided is not commensurate with the scope of the claim such that the narrowed range provides unexpected results in light of the combined teachings of Zhu et al. in view of Gupta. The comparative examples provided by the applicant does not help narrow the relative elemental ratios of Fe and Al since each example only has one dopant (i.e.: Fe or Al) (¶76 and ¶77 cited as US Pub. No. 2020/0235390 A1).
Based on the preceding discussion, the rejection of Claim 1 and dependent Claims 2 and 3 as being obvious primarily in light of Zhu et al. in view of Gupta et al. is maintained.
12. Regarding amended Claim 4, the rejection discussed in the first Office Action dated 14 July 2025 is maintained. Belharouak et al. (the primary reference for Claim 4) clearly teaches
a lithium metal oxide in different embodiments in ¶18-20, with the first embodiment having a range of compositions for Li1+wNixFeyAlzO2 (where 0≤w≤0.05, 0<x<1, 0<y≤0.2, 0<z≤0.2, and x+y+z=1). The method of synthesis taught by Belharouak et al. renders the limitations of amended Claim 4 as obvious as discussed above. While Belharouak et al. does not expressly disclose the OER activity of the Li1+wNixFeyAlzO2 materials, the modification of Belharouak et al. with Zhu et al. and Gupta et al. provides support for the inherent OER activity of the Li1+wNixFeyAlzO2 materials. The specific elemental composition ranges claimed in amended Claim 4 are also rendered obvious in light of Zhu et al. and Gupta et al. as explained in detail above.
Based on the preceding discussion, the rejection of Claim 4 and dependent Claim 5as being obvious primarily in light of Belharouak et al., Zhu et al., and Gupta et al. is maintained.
Conclusion
13. THIS ACTION IS MADE FINAL. 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.
14. Any inquiry concerning this communication or earlier communications from the examiner should be directed to KEVIN SYLVESTER whose telephone number is (703)756-5536. The examiner can normally be reached Mon - Fri 8:15 AM to 4:30 PM EST.
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/KEVIN SYLVESTER/Examiner, Art Unit 1794
/JAMES LIN/Supervisory Patent Examiner, Art Unit 1794