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 .
Response to Amendments
2. The response from the applicant dated 02 September 2025 has been entered into the record. The examiner acknowledges that Claims 1, 3, 5, 6, 7, 8, 9, 10, 11, 12, and 13 are currently pending. Claim 4 has been incorporated into Claim 1, meaning Claim 4 is cancelled. The examiner finds that the amendment has not introduced any new matter.
Claim Rejections - 35 USC § 103
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.
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.
3. Claims 1, 3, 5, 6, 7, 8, 9, 10, 11, 12, and 13 are rejected under 35 U.S.C. 103 as being unpatentable over Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al.
Adolphsen et al. (“Oxygen Evolution Activity and Chemical Stability of Ni and Fe Based Perovskites in Alkaline Media,” J. Electrochem. Soc. 2018, 165(10), F827-F835) is directed toward OER catalysts comprised of Perovskites (pg.: F827: title). Zhao et al. (“Vertical Growth of Porous Perovskite Nanoarrays on Nickel Foam for Efficient Oxygen Evolution Reaction,” ACS Sustainable Chem. Eng. 2020, 8, 4863−4870) is directed toward OER catalyst comprised of Perovskites on Ni foam (pg. 4863: abstract). Zhu et al. (“Perovskites decorated with oxygen vacancies and Fe–Ni alloy nanoparticles as high-efficiency electrocatalysts for the oxygen evolution reaction,” J. Mater. Chem. A 2017, 5, 19836-45) is directed toward the use of Fe-Ni alloy nanoparticles to improve the OER performance for Perovskite (pg. 19836: title and abstract).
Regarding Claim 1, Adolphsen et al. discloses a series of lanthanum-based Perovskite materials for use as catalysts in the oxygen evolution reaction in alkaline water (pg. F827: abstract). One compound having the formula La0.97Ni0.6Fe0.4O3 displayed a relatively low overpotential during the evaluation of OER of ~325 mV at 1 mA/cm2 (Figure 6). La0.97Ni0.6Fe0.4O3 can be rewritten in the form of formula (I) as: [(La)1]0.97(Ni)0.6(Fe)0.4O3 as per Claim 1 meaning that:
A is La and x =1, so there is no A’ is present in this compound since 1-x = 0;
y is 0.97;
B is Ni and B’ is Fe with z = 0.6 and 1-z = 0.4;
O is oxygen with δ = 0 since the subscript for oxygen is 3.
In order to calculate the SF parameter, a few terms must be specified based on the equation limitation claimed in Claim 1. The following parameters are listed in the table below and were used to calculate the SF for La0.97Ni0.6Fe0.4O3 which was 1.95. It has been held that a prima facie case of obviousness exists when an example disclosed in the prior art is within the claimed range. See MPEP 2144.05(I) - OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Table A. Parameters used to tabulate SF for La0.97Ni0.6Fe0.4O3
Compound
rA,av (angstroms)
rB,av (angstroms)
nA,av
r0(3- δ)/3
SF
La0.97Ni0.6Fe0.4O3
1.3192
0.556
2.91
1.35
1.95
Adolphsen et al. further discloses the use of a current collector made from gold used during electrochemical testing (pg. F828: electrochemical measurements section). However, Adolphsen et al. does not disclose a second material as part of the electrode as metallic nickel.
Zhao et al. discloses the deposition of a Perovskite material (LaCoO3) deposited onto nickel foam and sintered in Figures 1a, 1b, 1c, and 1d to form an electrode (pg. 4864). Zhao et al. indicates that the deposition of LaCoO3 improves the electrochemical performance relative to the bulk material as the OER overpotential is lower in the former case particularly at high potentials (pgs. 4866-7: Results and Discussion Section). Moreover, Zhao et al. discloses the deposition process of the LaCoO3 results in oxygen vacancies which are known to improve OER activity (pg. 4868: Results and Discussion Section). The improved catalytic activity of the Ni-foam supported LaCoO3 is a result of the good charge transfer ability of LaCoO3/NF ascribed to the uniform growth of porous LaCoO3 nanosheet on the conductive NF, which provides electron transfer pathways and superb electrical contact (Zhao on pg. 4868: Results and Discussion section).
It would be obvious to one of ordinary skill in the art prior to the effective filing date to modify the Au/Perovskite electrode disclosed in Adolphsen et al. by depositing the Perovskite (i.e.: La0.97Ni0.6Fe0.4O3) onto nickel foam in the manner taught by Zhao et al. with the reasonable expectation of forming an electrode with enhanced OER activity (Zhao on pg. 4868). Adolphsen et al. in view of Zhao et al. does not disclose the wherein the particles of ceramic material are immobilized and partly encapsulated by the second material.
Zhu et al. discloses the formation of oxygen vacancies and Fe-Ni alloy nanoparticles (i.e.: the second material) decorating (i.e.: partially encapsulating and immobilizing) the surface of the Perovskite material which is comprised of Fe and Ni (pg. 19837: introduction and pg. 19840: Figs. 4 and 5). The Fe-Ni nanoparticles are formed via an exsolution method by treating the precipitated and annealed Perovskite material with a reducing atmosphere of H2 or 5% H2 in argon as per pg. 18937 in the introduction and experimental/synthesis sections of Zhu et al. In Zhu et al., the formation of oxygen vacancies and Ni-Fe alloyed nanoparticles improves the OER electrochemical performance with results on par with iridium oxide (pg. 19841: results and discussion) and pg. 19844: conclusion).
It would be obvious to one of ordinary skill in the art to modify the surface of the ceramic material (e.g.: La0.97Ni0.6Fe0.4O3) on nickel foam as disclosed by Adolphsen et al. in view of Zhao et al. by treatment of the annealed electrode with a reducing (partial) hydrogen atmosphere as taught by Zhu et al. with the reasonable expectation of forming an electrode with improved OER performance due to the formation of oxygen vacancies and Ni-Fe alloyed nanoparticles. The electrode disclosed by the combination of Adolphsen et al. and Zhao et al. is capable of forming Ni-Fe nanoparticles on the surface of La0.97Ni0.6Fe0.4O3 because said ceramic material has both Ni and Fe present in the ceramic like the material disclosed in Zhu.
Regarding Claim 3, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode according to Claim 1 wherein the ceramic material of the formula (I) (e.g.: La0.97Ni0.6Fe0.4O3) is uniformly distributed onto the surface of the second material (e.g.: Ni foam) as evidenced by the SEM image and schematic from Zhao et al. showing the structure of the Perovskite material (LaCoO3) deposited onto nickel foam and sintered in Figures 1a, 1b, 1c, and 1d (pg. 4864).
Regarding Claim 5, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode according to Claim 1, wherein A is La, A’ is not present since x is 1 (so 1-x is 0) and wherein B is Ni and B’ is Fe as evidenced by the Perovskite compound La0.97Ni0.6Fe0.4O3 disclosed in Adolphsen et al. (pg. F827: abstract and pg. F831: Table 1).
Regarding Claim 6, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode according to Claim 1, wherein y is 0.97 as evidenced by the Perovskite compound La0.97Ni0.6Fe0.4O3 disclosed in Adolphsen et al. (pg. F827: abstract and pg. F831: Table 1).
Regarding Claim 7, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode as per Claim 1, wherein the average particle size of the ceramic material is between 10 and 300 nm as evidenced by the as evidenced by the SEM image and schematic from Zhao et al. showing the nano-structure of the Perovskite material (LaCoO3) deposited onto nickel foam and sintered in Figures 1d (pg. 4864).
Regarding Claim 8, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode as per Claim 1, wherein the ceramic material of the formula (I) has a Perovskite crystal structure as indicated on pg. 827 in the introduction (“Perovskite type materials”) and supported by XRD (pg. F829: Figure 1 “L97NF”).
Regarding Claim 9, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode according to Claim 1, wherein the electrode overpotential toward oxygen evolution reaction is less than or equal to 400 millivolts at a current density of 1 mA/cm2 as evidenced by Figure 6 on pg. F831 which shows the overpotential for La0.97Ni0.6Fe0.4O3 is ~325 mV at 1.0 mA/cm2. However, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. is silent on the OER overpotential at a current density of 1.0 mA/cm2 using a rotating disk electrode at a rotation rate of 1500 rpm in 20-35% KOH and at a temperature of 75-85 degrees Celsius.
According to at least the specification of the present application (cited as US App. No. 18/857384), ceramic materials that satisfy formula(I) which have intermediate SF values (i.e.: between 1.67 inclusive and 2.8 inclusive) simultaneously have inherently sufficient electrochemical activity (i.e.: low electrode overpotential toward OER) and inherently sufficient stability phase stability (pg. 5 lines 15-31). The instant application further clarifies sufficient electrochemical activity as an electrode overpotential towards oxygen evolution reaction is less than or equal to 400 mV at a current density of 1.0 mA/cm2, where the oxygen evolution reaction is carried out using a rotating disk electrode at a rotation rate of 1500 rpm in 20-35% KOH and at a temperature of 75-85 degrees Celsius (pg. 15 lines 26-34). Moreover, the specification of the instant application indicates that the aforementioned conditions are industrially relevant and has an OER overpotential on par with the state-of-the-art catalyst, IrO2 (pg. 16 lines 1-5).
Therefore, the combination of the ceramic material (e.g.: La0.97Ni0.6Fe0.4O3) having an SF value ranging from 1.67 inclusive to 2.8 inclusive (e.g.: SF = 1.95 for La0.97Ni0.6Fe0.4O3) on nickel foam (i.e.: the second material) would inherently have an oxygen evolution overpotential less than or equal to 400 millivolts at the claimed conditions as evidenced by, at least, the Applicant’s own disclosure (pg. 15 lines 26-34 to pg. 16 lines 1-5). See MPEP 2112-III.
Regarding Claim 10, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode according to Claim 1, wherein the ceramic material of formula (I) La0.97Ni0.6Fe0.4O3. Adolphsen et al. suggests that La0.97Ni0.6Fe0.4O3 and related compounds evaluated in the study could be used a OER catalysts at temperatures under 100 degrees Celsius (pg. F827: abstract). However, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. is silent on the phase-stability of ceramic compounds of formula (I) (e.g.: La0.97Ni0.6Fe0.4O3) in 6 M KOH at 80 degrees Celsius for 100 hours.
According to at least the specification of the present application (cited as US App. No. 18/857384), ceramic materials that satisfy formula(I) which have intermediate SF values (i.e.: between 1.67 inclusive and 2.8 inclusive) simultaneously have inherently sufficient electrochemical activity (i.e.: low electrode overpotential toward OER) and inherently sufficient stability phase stability (pg. 5 lines 15-31). The instant application further clarifies that sufficient phase stability is measured by exposure to 6 M KOH at 80 degrees Celsius for 100 hours (pg. 16 lines 14-24) and subsequent degradation analysis. According the specification of the instant application, ceramic materials lacking phase stability, that is those with SF value greater than 2.8, are not suitable for OER electrodes (pg. 17 lines 2-7).
Therefore, the combination of the ceramic material (e.g.: La0.97Ni0.6Fe0.4O3) having an SF value ranging from 1.67 inclusive to 2.8 inclusive (e.g.: SF = 1.95 for La0.97Ni0.6Fe0.4O3) on nickel foam (i.e.: the second material) would inherently be phase stable in 6 M KOH at 80 degrees Celsius for 100 hours as evidenced by, at least, the Applicant’s own disclosure (pg. 15 lines 26-34 to pg. 16 lines 1-5). See MPEP 2112-III.
Regarding Claim 11, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses the electrode according to Claim 1, wherein the SF value is 1.95 (as calculated above). It has been held that a prima facie case of obviousness exists when an example disclosed in the prior art is within the claimed range. See MPEP 2144.05(I) - OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 12, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses an alkaline electrolysis stack (1 M KOH as per the abstract on pg. F827 of Adolphsen et al.) comprising at least one electrode according to Claim 1 as evidenced by Adolphsen et al. on pg. F828 in the electrochemical measurements section where the electrochemical activity was evaluated using a three-electrode set up with the La0.97Ni0.6Fe0.4O3 (gold or nickel-foam) as the working electrode. Adolphsen et al. further discloses a platinum mesh/wire is the counter electrode (to produce hydrogen from water splitting) on pg. F828 (electrochemical measurements section).
Regarding Claim 13, Adolphsen et al. in view of Zhao et al. and further in view of Zhu et al. discloses a method for water electrolysis of water in alkaline conditions using the alkaline electrolysis stack according to Claim 12 as indicated in Adolphsen at al. in the following areas: the abstract on pg. F827, electrochemical measurements section on pg. F828, and the electrochemical activity toward the OER section on pgs. F828-30.
Response to Arguments
4. The examiner agrees with that applicant as per their response on pg. 5-8 that the combination for Adolphsen et al. and Zhao et al. does not teach the limitations of amended Claim 1. However, amended Claim 1 was written by incorporating Claim 4 into Claim 1 both from the claim set dated 27 March 2025. Claim 4 from the claim set dated 27 March 2025 was rejected as being obvious over the combination of Adolphsen et al., Zhao et al. and Zhu et al. Therefore, amended Claim 1 is rejected under 103 as being obvious in light of the combination of Adolphsen et al., Zhao et al. and Zhu et al.
5. Dependent Claims 3, 5, 6, 7, 8, 9, 10, 11, 12, and 13 are also rejected under 103 in view of the combination of Adolphsen et al., Zhao et al. and Zhu et al.
6. Given the mathematical formula for the determination of the stability factor described by the applicant in at least amended Claim 1, said stability factor is solely directed by the stoichiometry of the ceramic material. In other words, the input variables to calculate the stability factor are based on fundamental properties pertaining to the elements in the ceramic material (e.g.: perovskite), such as Shannon ionic radii and oxidation state. Therefore, the stability factor is a calculated value that is inherent to a specific ceramic of a given elemental composition or molecular formula. Provided a ceramic material has a value within the claimed range for stability factor (e.g.: 1.67 to 2.8) and meets the compositional limitation (i.e.: molecular formula) of amended Claim 1, said ceramic material will have the capacity to carry out the oxygen evolution reaction, regardless of the method of formation (e.g.: wet chemical synthesis, solid phase synthesis, CVD, etc.). If the applicant wishes to draw a distinction between method of synthesis of the ceramic material (and the second material), these limitations should be explicitly included in the claim limitations. The applicant is reminded that 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).
7. On pg. 6-7, the applicant has further argued that the perovskite formation method described in Zhao et al. (i.e.: wet chemical synthesis) would not be applicable to the composition described by Adolphsen et al. since Adolphsen’s composition (e.g.: La0.97Ni0.6Fe0.4O3) is prepared by combustion spray pyrolysis followed by a high temperature annealing step. However, the examiner disagrees with the applicant’s contention that the method of Zhao et al. would not be capable of forming the composition of Adolphsen. In fact, Jia et al. (“Weakening the strong Fe-La interaction in A-site-deficient perovskite via Ni substitution to promote thermocatalytic synthesis of carbon nanotubes from plastics,”
J. Hazard. Mater. 2021, 403, article 123642, pg. 1-11) and Shah et al. (“The effects of stoichiometry on the properties of exsolved Ni-Fe alloy nanoparticles for dry methane reforming,” AIChE J. 2020, 66, article e17078, pg. 1-12). provide clear support for the formation of lanthanum deficient nickel iron oxides using solution methods (Jia et al. on pg. 2: 2.1. Sample Preparation – La0.8NixFe1-xO3-d and Shah et al. on pg. 2: 2.1 Catalyst preparation - La0.9Ni0.1Fe1O3-d). In these two references, the stoichiometry of the perovskite material (e.g.: La0.8NixFe1-xO3-d or La0.9Ni0.1Fe1O3-d) is set by the stoichiometry in the precursor solution. Moreover, both of these references indicate that annealing the resultant gel material from the wet chemical under a reducing atmosphere of hydrogen results in the formation of Ni/Fe nanoparticles. This finding is in agreement with the Zhu et al. which seems to require a reducing atmosphere of H2 or H2 in argon to form the metallic nanoparticles via exsolvation.
8. The applicant has alleged that the formation of Ni/Fe nanoparticles on the surface of a ceramic material via exsolvation is not equivalent to the “partially encapsulating and immobilizing.” However, the examiner disagrees with this interpretation because partially covering the surface of a ceramic material (e.g.: perovskites like La0.97Ni0.6Fe0.4O3) with a nanoparticle (e.g.: Ni/Fe alloy) would both partially encapsulate and immobilize the ceramic material from interactions between adjacent nanoparticles.
9. The applicant has also argued on pg. 8-9 that the formation reduces the activity of the ceramic material toward oxygen evolution reaction. The examiner disagrees with these assertions as Ni and/or Fe nanoparticles are well-known OER catalysts and are capable of providing the added benefit of electrical conductivity (as they are metallic) that many ceramic materials lack.
Conclusion
10. 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.
11. 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