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 amendment dated 15 October 2025 has been entered into the record. The examiner agrees with the applicant that the amendment has not introduced any new matter. Currently, Claims 1, 2, 3, 4, 5, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, and 18 are pending. Claim 18 is new and Claims 6 and 7 were cancelled by the applicant.
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, 2, 3, 4, 5, 8, 9, and 18 are rejected under 35 U.S.C. 103 as being unpatentable over Jörissen et al. in view Ali Ehsan et al.
Jörissen et al. (US Pub. No. 2021/0079539 A1 – previously presented) is directed toward a nickel electrode, method for manufacturing the same, and use thereof (title). Ali Ehsan et al. (“Facile and scalable fabrication of nanostructured nickel thin film electrodes for electrochemical detection of formaldehyde,” Anal Methods 2020, 12, 4028-4036 – previously presented) is directed toward an electrocatalyst comprising a metallic nickel layer (pg. 4028: abstract).
Regarding Claim 1, Jörissen et al. discloses a nickel electrode that has a layer of mutually adherent, spherical nickel particles applied to support with inner surface area such as foam electrodes (¶27). Jörissen et al. further indicates that “nanostructured” nickel meshes or nickel expanded metals are used for alkaline water electrolysis (i.e.: OER) because of their high surface area and low electrical resistance (¶28-30). The method of Jörissen et al. results in the formation of metallic nickel particles (on nickel foam) with an example having a mean particle size of 3.4 µm (TABLE 1 in ¶69), but a broader particle size range of 0.1 to 25 µm (¶54) is also disclosed. One of ordinary skill in the art would be motivated to decrease the average particles size of the nickel particles to improve the catalytic activity owing to the higher surface area of smaller particles leading to a higher concentration of catalytically active sites.
Ali Ehsan et al. is directed toward the formation of an oxidation electrocatalyst comprising a metallic nickel layer (pg. 4028: abstract). Ali Ehsan et al. indicates that metallic nickel films and layers can be deposited using AACVD when specifically Ni(acac)2 is the nickel precursor (pg. 4030: Results) as other derivatives of acetylacetone ligands, “acac,” form nickel oxide. Ali Ehsan et al. further discloses the metallic nickel particles form a continuous layer on the (FTO) substrate as explained in section 3.1 (Structural analysis of nickel films) where increasing the reaction time from 10 to 40 minutes improved the quality, coverage, cohesion, and adhesion of the nickel film. In fact, Ali Ehsan et al. indicates that after 10 minutes the uniformly deposited Ni nanoparticles begin to agglomerate and at a reaction time of 40 minutes clusters (analogous to “aggregates” of the instant application). Given the description as nanoparticles in Ali Ehsan, the limitation of the average particle size diameter of Claim 1 is met (i.e.: an average ranging from 100-500 nm). Moreover, Claim 1 also requires that the average diameter of each aggregate ranges between 0.5 and 5 microns. The average diameter of the aggregates as per Ali Ehsan et al. is ~1 micron based on the SEM image in Fig. 2C and Fig. 2D (pg. 4030).
Jörissen et al. in view of Ali Ehsan et al. further discloses the electrocatalyst is comprised of metallic nickel particles that form a continuous layer on the nickel foam substrate as explained in section 3.1 (Structural analysis of nickel films) of Ali Ehsan et al. whereby increasing the reaction time from 10 to 40 minutes the film's quality, coverage, cohesion, and adhesion all improved. The combination of references also teaches the layer of metallic nickel particles on the nickel foam substrate has a thickness of 20 to 200 μm (Jörissen et al. in ¶53) which can be achieved by changing the deposition time during AACVD as indicated by Ali Ehsan et al (Ali Ehsan et al. on pg. 4031: 3.1 Structural analysis of nickel films section).
It has been held that a prima facie case of obvious exists when the claimed range overlaps or lies within ranges disclosed by the prior art. See MPEP 2144.05(I) - OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
It would be obvious to one of ordinary skill in the art prior to effective filing date of the claimed invention to prepare the nickel coated nickel foam taught by Jörissen et al. using Ali Ehsan’s AACVD method to prepare a metallic layer of nickel nanoparticles with the reasonable expectation of forming a more active OER catalyst owing to the increase in surface area of nickel nanoparticles (from Ali Ehsan et al.) over nickel microparticles (from Jörissen et al.).
Regarding Claim 2, Jörissen et al. in view of Ali Ehsan et al. discloses an electrocatalyst as per Claim 1, wherein the aggregates of the metallic nickel particles have a popcorn shape as depicted in Fig. 2a and Fig. 2b below. (Ali Ehsan et al. on pg. 4030).
[AltContent: textbox ([img-media_image1.png]
FIG. 2a and 2b. from Ali Ehsan et al. showing structure of deposited nickel film after 10 and 20 minutes (pg. 4030).)]
On page 12 of the instant applicant’s specification, popcorn shape refers to “a single center particle with multiple other particles random(ly) dispersed on its surface” (Lines 13-17). FIG. 2F from the instant application is reproduced to depict a visual meaning of “popcorn shape.” The SEM images from Ali Ehsan et al. and the instant application (FIG. 2F) depict similar morphologies that meet the definition of “popcorn shape” as defined by the applicant from the instant application (pg. 12: Lines 13-17).
[AltContent: textbox ([img-media_image2.png]
FIG. 2F from the instant application showing aggregates with a “popcorn shape”)]
Regarding Claim 3, Jörissen et al. in view of Ali Ehsan et al. discloses the electrocatalyst of Claim 1, wherein the metallic nickel particles have a cubic crystal structure as indicated by XRD analysis (Ali Ehsan et al. on pgs. 4030-1: 3.1 Structural analysis of nickel films section).
Regarding Claim 4, Jörissen et al. in view of Ali Ehsan et al. discloses the electrocatalyst of Claim 1, wherein the metallic nickel particles comprise Ni0 (Ali Ehsan et al. on pgs. 4030-1: 3.1 Structural analysis of nickel films section).
Regarding Claim 5, Jörissen et al. in view of Ali Ehsan et al. discloses the electrocatalyst of Claim 1, wherein at least 90% of an outer surface area of the nickel foam substrate is covered with the layer of metallic nickel as evidenced by the SEM images from Ali Ehsan et al. showing structure of deposited nickel film after 10 and 20 minutes (pg. 4030). The film is nickel as indicated by Ali Ehsan et al. on pg. 4029 in section 2.1 Fabrication of metallic nickel film electrodes. It has been held that a prima facie case of obvious exists when the claimed range overlaps or lies within ranges disclosed by the prior art. See MPEP 2144.05(I) - OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 8, Jörissen et al. in view of Ali Ehsan et al. discloses the electrocatalyst of Claim 1, wherein the nickel foam substrate is porous and has an average pore size of 50 to 500 microns as evidenced by FIG. 2 from Jörissen et al. depicted below and explained in ¶60. It has been held that a prima facie case of obvious exists when the claimed range overlaps or lies within ranges disclosed by the prior art. See MPEP 2144.05(I) - OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 9, Jörissen et al. in view of Ali Ehsan et al. discloses the electrocatalyst of Claim 8, wherein the pores have a spherical shape as supported by the SEM image from Jörissen et al. (¶60 and FIG. 2).
[AltContent: textbox ( [img-media_image3.png]
FIG. 2 from Jörissen et al. showing pore size and shape of commercial nickel foam relevant to Claim 8 and 9 of the instant application)]
Regarding Claim 18, Jörissen et al. and Ali Ehsan et al. discloses the electrocatalyst of Claim 1, wherein the metallic nickel particles form a continuous layer having a thickness of 0.1 to 10 microns on the nickel foam substrate. As explained above in Claim 1, Jörissen et al. and Ali Ehsan et al. teach a film thickness ranging from 20 to 200 microns, which is an approaching range, amount, or proportion resulting in a prima facie case of obviousness (See MPEP 2144.05(I).
Alternatively pertaining to Claim 18, Jörissen et al. and Ali Ehsan et al. disclose the layer thickness of 0.1 to 10 microns as part of routine optimization. As explained above in Claim 1, Ali Ehsan indicates that the thickness of the film can be controlled by the deposition time (using AACVD) and the average diameter of the aggregates as per Ali Ehsan et al. is ~1 micron based on the SEM image in Fig. 2C and Fig. 2D (pg. 4030). Combining the thickness controlled by deposition time and the ~1 micron particle diameter of the AACVD deposited particles allows for reducing the film thickness closer to the specific range of Claim 18 as part of routine optimization. Therefore, the layer thickness 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 layer thickness, including values within the claimed range, through routine experimentation. One would have been motivated to do so in order to have a layer of sufficient thickness to allow effective catalytic activity (i.e.: high concentrations of catalytic species) and allow facile electron transfer between the metallic (Ni) layer and the nickel foam substrate during catalytic reactions.
4. Claims 10, 11, 12, 13, 14, 15, 16, and 17 are rejected under 35 U.S.C. 103 as obvious over Jörissen et al. in view of Ali Ehsan as applied to Claim 1 and further in view of Peugeot et al.
Jörissen et al. (US Pub. No. 2021/0079539 A1) is directed at a nickel electrode, method for manufacturing the same, and use thereof (title). Ali Ehsan et al. (“Facile and scalable fabrication of nanostructured nickel thin film electrodes for electrochemical detection of formaldehyde,” Anal Methods 2020, 12, 4028-4036) is directed toward an electrocatalyst comprising a metallic nickel layer (pg. 4028: abstract). Peugeot et al. (US Pub. No. 2024/0328005 A1 – foreign priority date of 18 October 2021) is directed toward an OER electrode catalyst assembly comprising dendritic nickel foam (title).
Regarding Claim 10, Jörissen et al. in view of Ali Ehsan et al. discloses the electrocatalyst of Claim 1 indicating that the electrode can be used for water electrolysis (i.e.: “oxidation of water”), but does not provide specific details on said process (abstract and ¶1). Peugeot et al. discloses an electrocatalyst (i.e.: oxygen evolution catalyst in the title and abstract) comprising: a nickel foam substrate (abstract, ¶13-24, ¶190-1, Example 1) and a layer of metallic nickel particles on the foam substrate deposited via electrodeposition (abstract, ¶13-24, ¶190-1, and Example 1). Jörissen et al. in view of Ali Ehsan et al. also discloses an electrocatalyst comprised of metallic nickel deposited onto nickel foam as explained in detail for Claim 1 above. Therefore, Jörissen et al. in view of Ali Ehsan et al. and Peugeot et al. are both directed toward the same composition and the same field of endeavor.
Further pertaining to Claim 10, Peugeot et al. specifically discloses a method of oxidizing water, comprising contacting a metallic nickel layer on nickel foam electrocatalyst and a counter electrode (platinum mesh) with the water (1 M aqueous KOH) as indicated in ¶176. The method according to Peugeot et al. also comprises applying a potential (vs. the RHE) to the electrocatalyst, wherein the electrocatalyst (nickel particles on nickel foam) and the counter electrode (platinum mesh) are at least partially submerged in the water and not in physical contact with each other as the electrochemical cell in Peugeot et al. has two compartments separated by a glass frit (¶176).
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 catalyst composition described in the combination of Jörissen et al. in view of Ali Ehsan et al. (i.e.: the electrocatalyst of Claim 1) as the electrocatalyst in the method of oxidizing water taught by Peugeot et al. with the reasonable expectation of forming a highly active electrocatalyst owing to the increase in surface area of nickel nanoparticles (from Ali Ehsan et al.) over nickel microparticles (from Jörissen et al.).
Regarding Claim 11, Jörissen et al. and Ali Ehsan et al. in view of Peugeot et al. discloses the method of Claim 10, wherein the water is an aqueous electrolyte solution with a base that is an alkali metal hydroxide as indicated in ¶176 of Peugeot et al. by the use of aqueous 1 M potassium hydroxide electrolyte.
Regarding Claim 12, Jörissen et al. and Ali Ehsan et al. in view of Peugeot et al. discloses the method of Claim 11, wherein the base in potassium hydroxide (i.e.: aqueous 1 M KOH) as indicated in ¶176 of Peugeot et al.
Regarding Claim 13, Jörissen et al. and Ali Ehsan et al. in view of Peugeot et al. discloses the method of Claim 10, wherein the counter electrode is made of platinum by the use of platinum mesh as the counter electrode (Peugeot et al. in ¶176).
Regarding Claim 14, Jörissen et al. and Ali Ehsan et al. in view of Peugeot et al. discloses the method of Claim 10 using the electrocatalyst of Claim 1, but does explicitly measure the water oxidation overpotential. The electrocatalyst in the instant application (and Claim 1) has a water oxidation potential of 280-305 mV as indicated on pg. 15 lines 14-15 of the specification. Therefore, the electrocatalyst of Claim 1 described by Jörissen et al. and Ali Ehsan et al. used in the method of water oxidation of Peugeot et al. used in Claim 14 would inherently have a water oxidation overpotential of 280-305 mV as evidenced by, at least, the Applicant’s own disclosure (pg. 15 lines 14-15). See MPEP 2112-III.
Regarding Claim 15, Jörissen et al. and Ali Ehsan et al. in view of Peugeot et al. discloses the method of Claim 14, only measuring the water oxidation over potential for less than one hour (using the electrocatalyst of Claim 1) as indicated in ¶179 of Peugeot et al. Thus, the combination of references is silent on the overpotential measurement variation after 10-50 hours. The electrocatalyst in the instant application (and Claim 1) has a water oxidation potential of 280-305 mV as indicated on pg. 15 lines 14-15 of the specification and the specification further indicates that said overpotential does not vary by more than 5% after the potential is applied for 10-50 hours (pg. 15 lines 15-17). Therefore, the electrocatalyst of Claim 1 described by Jörissen et al. and Ali Ehsan et al. used in the method of water oxidation of Peugeot et al. used in Claim 14 would inherently have a water oxidation overpotential does not vary by more than 5% after the potential is applied for 10-50 hours as evidenced by, at least, the Applicant’s own disclosure (pg. 15 lines 15-17). See MPEP 2112-III.
Regarding Claim 16, Jörissen et al. and Ali Ehsan et al. in view of Peugeot et al. discloses the method of Claim 10, but does not specify the electrochemically active surface area (ESCA). The electrocatalyst in the instant application (and Claim 1) has an ESCA of 250-300 centimeter square (cm2) as indicated on pg. 15 lines 20-23 of the specification. Therefore, the electrocatalyst of Claim 1 described by Jörissen et al. and Ali Ehsan et al. used in the method of water oxidation of Peugeot et al. used in Claim 10 would inherently have an ESCA of 250-300 centimeter square (cm2) as evidenced by, at least, the Applicant’s own disclosure (pg. 15 lines 20-23). See MPEP 2112-III.
Regarding Claim 17, Jörissen et al. and Ali Ehsan et al. in view of Peugeot et al. discloses the method of Claim 10 which uses the electrocatalyst of Claim 1 only evaluating voltages less than 1.6 V (FIG. 8B only showing the current density response at less than 0.5 V). Thus, the combination of reference is silent on the current density response of the electrocatalyst at 1.6 V. The electrocatalyst in the instant application (and Claim 1) has a water oxidation potential of 280-305 mV as indicated on pg. 15 lines 14-15 of the specification and the specification further indicates that said electrocatalyst has a current density of at least 1,000 mA cm-2 at 1.6 V (pg. 15 line 23 to pg. 16 lines 1-2). Therefore, the electrocatalyst of Claim 1 described by Jörissen et al. and Ali Ehsan et al. used in the method of water oxidation of Peugeot et al. used in Claim 10 would inherently have a current density of at least 1,000 mA/cm2 at 1.6 V as evidenced by, at least, the Applicant’s own disclosure (pg. 15 line 23 to pg. 16 lines 1-2). See MPEP 2112-III.
Response to Arguments
5. The applicant has argued that the rejection of Claim 1 as being anticipated by either Fontecave et al. or Peugeot et al. has been overcome by the amendment to Claim 1 where Claims 6 and 7 were added as new limitations. The examiner generally agrees with this argument presented on pg. 5-6 of the applicant’s response that the two previous references do not explicitly teach a continuous film and the previous rejections have been withdrawn.
6. The applicant’s arguments on pg. 6-9 pertaining to the 103 rejection of amended Claim 1 in view of Jörissen et al. and Ali Ehsan et al. were considered and are not persuasive. The applicant has amended Claim 1 to include Claims 6 and 7, which were previously rejected under 103 as being obvious in light of Jörissen et al. and Ali Ehsan et al. as indicated in the first Office Action dated 15 July 2025.
7. Claims 1, 2, 3, 4, 5, 8, 9, and 18 are rejected under 103 as being obvious in light of Jörissen et al. and Ali Ehsan et al. Claims 10, 11, 12, 13, 14, 15, 16, and 17 are rejected under 103 as being obvious in light of Jörissen et al. and Ali Ehsan et al. and further in view of Peugeot et al. See the above office action for further details.
8. The applicant has argued that the rationale for the combination of Jörissen et al. and Ali Ehsan et al. was not explained by the examiner in the previous office Action on pg. 6-8 of their response. However, the examiner disagrees with this assessment as it was previously explained that the nickel layer deposited onto a nickel foam in both Jörissen et al. and Ali Ehsan et al. are both compositions that are capable of being directed at catalytically oxidative reactions. Since both of these compositions are similar and are directed toward oxidative processes, combination of teachings from both references would be obvious to one of ordinary skill in the art. Moreover, the teachings of only Jörissen et al. and Ali Ehsan et al. were applied to claims (i.e.: Claims 1, 2, 3, 4, 5, 8, 9, and 18) that did not specify a certain type of catalytic reaction (e.g.: water oxidation as is a required limitation for Claims 10-17), but the combination of references did indicate that nickel electrocatalyst were useful for oxidatively catalytic process. In order to address the specific method of water oxidation, which is a required limitation of Claims 10-17, the examiner included the teachings of Peugeot et al. which explicitly teaches a method of water oxidation that uses a similar composition to Jörissen et al. and Ali Ehsan et al., i.e.: a metallic nickel layer deposited onto a porous nickel substrate.
Conclusion
9. 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.
10. 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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If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, James Lin can be reached at 571-272-8902. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300.
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/KEVIN SYLVESTER/Examiner, Art Unit 1794 /JAMES LIN/Supervisory Patent Examiner, Art Unit 1794