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 applicant’s response filed 29 December 2025 has been entered into the record and is considered fully responsive. The applicant has cancelled Claims 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 22, and 23. The applicant has added new Claims 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, and 41. Claims 20, 21, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, and 41 are pending and under examination.
Claim Rejections - 35 USC § 103
3. 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.
4. 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.
5. Claims 20, 21, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, and 41 are rejected under 35 U.S.C. 103 as being unpatentable over Liu et al. and Jesswein.
Liu et al. (CN111420676A – EPO Translation; previously presented) is directed at inorganic-organic hybrid metal particles for water splitting (title and abstract). Jesswein (DE102012223556A1 – EPO translation) is directed toward application of a conductive paste and subsequent sintering (title).
Based on the applicant’s amendment and new claims, Claim 20 and Claim 33 are now the independent claims.
Regarding Claim 20, Liu et al. discloses a method making an electrode, comprising: contacting a substrate (e.g.: nickel foam) with a formulation comprising an electrode material comprising a plurality of polyacrylic acid (PAA) coated silver nanoparticles (synthesis of PAA-AgNPs disclosed in ¶11-23) as described in examples in ¶44, 48, and 57. The general procedure disclosed by Liu et al. indicates that the nickel foam immersed in the PAA-AgNPs dispersion and then removed followed by drying at 60 to 80 °C for 4 to 8 hours, and then calcining at 300 to 600 °C for 2 to 3 hours under argon protection to obtain an electrocatalytic water splitting catalyst (¶27). The resultant catalyst is composed of a carbonized layer embedded with silver metallic particles loaded on the surface of the nickel foam (¶27). Argon is explicitly used to protection the electrocatalytic water splitting catalyst by excluding oxygen and allowing carbonization of the organic species (i.e.: PAA) during sintering at temperatures above 300 °C.
A prima facie case of obviousness exists when the sintering temperature range disclosed in the prior art (300 to 600 °C) overlaps with the claimed sintering temperature range (150 to 700 °C) as in Claim 20. See MPEP 2144.05(I) – OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS
Pertaining to the amendment to Claim 20, Liu et al. does not expressly indicate whether the application/depositing of the silver paste to the substrate occurs under an inert or reducing atmosphere (i.e.: hydrogen). Jesswein discloses the application of a conductive paste with (Ag) nanoparticles in the submicron range with a range of 10-50 nm (¶9) meaning Jesswein is analogous art to Liu et al. Jesswein further discloses that application and optionally drying of oxidation prone metallic nanoparticle pastes (i.e.: silver and copper) takes place under an inert (or reducing atmosphere) to prevent the surface oxidation of the conductive paste (¶12).
Therefore, the use of an inert atmosphere during the application process as per Jesswein and the use of an argon atmosphere during the sintering process of Liu et al. serve the same purpose of preventing oxidation of the silver nanoparticles at the surface of the deposited/annealing conductive ink. Combination of these two references would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention with the reasonable expectation of preventing Ag surface oxidation during the entire Ag-electrode formation process.
Moreover, the present application indicates that on pg. 10 in ¶47 of the disclosure that: “by maintaining a hydrogen atmosphere, oxidation of the top surface of the substrate is avoided. In embodiments, the ink or paste may be deposited or printed atop or directly atop various substrates to form an electrode.” Thus, showing the use of argon/inert atmosphere in Jesswein/Liu et al. serves the same purpose as the use of hydrogen in the present application during the deposition and annealing processes, that is, removal of oxygen exposure.
It would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention that an inert atmosphere (e.g.: art) as taught by Liu et al. and Jesswein and a hydrogen atmosphere as in the instant application maintained during the depositing and annealing steps protect the silver from oxidizing in the presence of oxygen indicating they are equivalent steps in the art known for the same process. See MPEP 2144.06(II) – Art Recognized Equivalence for the Same Purpose: Substituting Equivalent Known for the Same Purpose.
Regarding Claim 21, Liu et al. in view of Jesswein discloses the method of Claim 20, wherein the electrode material comprising a plurality of PAA coated silver nanoparticles is provided in an amount sufficient to form a continuous layer as evidenced by immersing the nickel foam into the PAA-AgNPs dispersion, subsequently drying and carbonizing the film under argon atmosphere to make the supported catalyst cathode made of silver particles embedded in a carbon layer loaded onto nickel foam (Liu et al. in ¶26-27, ¶42-44, ¶47-48, and ¶56-57).
Regarding Claim 24, Liu et al. in view of Jesswein discloses the method of Claim 20, wherein the plurality of PAA coated silver nanoparticles have an average longest diameter of between 1-30 nm as evidenced by the average diameter of the AgNPs of ~2-5 nm (Liu et al. in ¶24 and 27). Since the nanoparticles are spherical (with support from an SEM image showing Au particles in FIG. 1 of Liu et al.), the longest diameter and the diameter of said nanoparticles are the same. It has been held that a prima facie case of obviousness exists when the range disclosed in the prior art overlaps with the claimed range. See MPEP 2144.05(I) – OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 25, Liu et al. in view of Jesswein discloses the method of Claim 20, wherein the plurality of PAA coated silver nanoparticles (“AgNPs@PAA”) are characterized as substantially mono-disperse nanoparticles having an average diameter of about 1.0 to 30 nm as indicated in ¶24 and 27 of Liu et al. where the average diameter of the AgNPs is ~2-5 nm. It has been held that a prima facie case of obviousness exists when the range disclosed in the prior art overlaps with the claimed range. See MPEP 2144.05(I) – OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 26, Liu et al. in view of Jesswein discloses the method of Claim 20, wherein the plurality of PAA coated silver nanoparticles (“AgNPs@PAA”) are characterized as substantially mono-disperse nanoparticles having an average diameter of about 1.0 to 10 nm as indicated in ¶24 and 27 of Liu et al. where the average diameter of the AgNPs is ~2-5 nm. It has been held that a prima facie case of obviousness exists when the range disclosed in the prior art overlaps with the claimed range. See MPEP 2144.05(I) – OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 27, Liu et al. in view of Jesswein discloses the method of Claim 20, wherein the plurality of PAA coated silver nanoparticles (“AgNPs@PAA”) are characterized as electrocatalysts toward hydrogen evolution in acidic media as indicated in ¶31 and 32 of Liu et al. where the catalytic HER performance is termed “excellent.” During the evaluation of HER activity, Liu et al. uses a 0.5 M H2SO4 electrolyte, which is acidic media (¶50 and 59).
Regarding Claim 28, Liu et al. in view of Jesswein discloses the method of Claim 20, but is silent on the altered crystal structure featuring a lower surface of atomic coordination number nor a lattice strain of about 0.5% to about 1% of the plurality of particles. The specification of the instant application indicates that in certain embodiments, the plurality of particles have a lower surface atomic coordination number on page 8 in ¶39 and that increasing the surface area of Ag results in more unsaturated coordination atoms on page 2 thereby improving the HER activity of said catalyst. Liu et al. discloses the electrode material Claim 20 which comprises PAA-coated silver nanoparticles which have increased surface area from the small particle size (2-5 nm diameter) and catalyze the HER reaction. Therefore, the electrode material of Claim 20 would inherently have an altered crystal structure featuring a lower surface of atomic coordination number as evidenced by, at least, the Applicant’s own disclosure (pg. 2 in ¶6 and pg. 8 ¶39). See MPEP 2112-III.
Regarding Claim 29, Liu et al. in view of Jesswein discloses the method of Claim 20, wherein the electrode material is characterized as a catalyst (toward hydrogen evolution reaction) as per ¶31 and 32 in Liu et el.
Regarding Claim 30, Liu et al. in view of Jesswein discloses the method of Claim 20, comprising a capping agent which is analogous to the aqueous polymer of Liu et al. (¶15 and 16). The aqueous polymer controls the size of the Ag particles, provides stability to the silver particles, coats the nanoparticles, and binds them into super particles (¶22, 24, 27, and 29).
Regarding Claim 31, Liu et al. in view of Jesswein discloses the method of Claim 20, but does not explicitly disclose the use of a carbon-based substrate (or electrode support). Nickel foam is a high surface area conductive material, but is susceptible to dissolution or leaching of nickel ions into the acidic electrolyte (e.g.: 0.5 M sulfuric acid). The presence of dissolved nickel ions can scavenge the electrons that are used to reduce protons to hydrogen gas during the hydrogen evolution reaction, thereby lowering the catalytic efficiency of the PAA-nano-silver electrode material. Conversely, glassy carbon supports (electrodes) are conductive and resistant to acid electrolytes. It would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention to substitute a glassy carbon electrode for the nickel foam support disclosed by Liu et al. in view of Jesswein with the reasonable expectation of increasing the catalytic efficiency of the PAA-AgNPs for hydrogen evolution reaction. See MPEP 2144.06(II) – Art Recognized Equivalence for the Same Purpose: Substituting Equivalent Known for the Same Purpose.
Regarding Claim 32, Liu et al. in view of Jesswein discloses the method of Claim 20, further comprising preventing oxidation of the top surface of substrate during the depositing and the heating as supported by ¶27 in Liu et al. and ¶12 in Jesswein since both processes occur under an inert/reducing atmosphere (i.e.: non-oxidizing).
Regarding Claim 33, Liu et al. discloses an electrode made by a process comprising: depositing a formulation onto a substrate where the substrate is nickel foam and the formulation is polyacrylic acid (PAA) coated silver nanoparticles (synthesis of PAA-AgNPs disclosed in ¶11-23) as described in examples in ¶44, 48, and 57 used to form the electrode material. The general procedure disclosed by Liu et al. indicates that the nickel foam immersed in the PAA-AgNPs dispersion and then removed followed by drying at 60 to 80 °C for 4 to 8 hours, and then calcining at 300 to 600 °C for 2 to 3 hours under argon protection to obtain an electrocatalytic water splitting catalyst (¶27). The resultant catalyst is composed of a carbonized layer embedded with silver metallic particles loaded on the surface of the nickel foam (¶27). Argon is explicitly used to protection the electrocatalytic water splitting catalyst by excluding oxygen and allowing carbonization of the organic species (i.e.: PAA) during sintering at temperatures above 300 °C.
A prima facie case of obviousness exists when the sintering temperature range disclosed in the prior art (300 to 600 °C) overlaps with the claimed sintering temperature range (150 to 700 °C) as in Claim 20. See MPEP 2144.05(I) – OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS
However, Liu et al. does not expressly indicate whether the application/depositing of the silver paste to the substrate occurs under an inert or reducing atmosphere (i.e.: hydrogen). Jesswein discloses the application of a conductive paste with (Ag) nanoparticles in the submicron range with a range of 10-50 nm (¶9) meaning Jesswein is analogous art to Liu et al. Jesswein further discloses that application and optionally drying of oxidation prone metallic nanoparticle pastes (i.e.: silver and copper) takes place under an inert (or reducing atmosphere) to prevent the surface oxidation of the conductive paste (¶12).
Therefore, the use of an inert atmosphere during the application process as per Jesswein and the use of an argon atmosphere during the sintering process of Liu et al. serve the same purpose of preventing oxidation of the silver nanoparticles at the surface of the deposited/annealing conductive ink. Combination of these two references would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention with the reasonable expectation of preventing Ag surface oxidation during the entire Ag-electrode formation process.
Moreover, the present application indicates that on pg. 10 in ¶47 of the disclosure that: “by maintaining a hydrogen atmosphere, oxidation of the top surface of the substrate is avoided. In embodiments, the ink or paste may be deposited or printed atop or directly atop various substrates to form an electrode.” Thus, showing the use of argon/inert atmosphere in Jesswein/Liu et al. serves the same purpose as the use of hydrogen in the present application during the deposition and annealing processes, that is, removal of oxygen exposure.
It would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention that an inert atmosphere (e.g.: art) as taught by Liu et al. and Jesswein and a hydrogen atmosphere as in the instant application maintained during the depositing and annealing steps protect the silver from oxidizing in the presence of oxygen indicating they are equivalent steps in the art known for the same process. See MPEP 2144.06(II) – Art Recognized Equivalence for the Same Purpose: Substituting Equivalent Known for the Same Purpose.
Regarding Claim 34, Liu et al. in view of Jesswein discloses the electrode of Claim 33, wherein the electrode material comprising a plurality of PAA coated silver nanoparticles is provided in an amount sufficient to form a continuous layer as evidenced by immersing the nickel foam into the PAA-AgNPs dispersion, subsequently drying and carbonizing the film under argon atmosphere to make the supported catalyst cathode made of silver particles embedded in a carbon layer loaded onto nickel foam (Liu et al. in ¶26-27, ¶42-44, ¶47-48, and ¶56-57).
Regarding Claim 35, Liu et al. in view of Jesswein discloses the electrode of Claim 33, wherein the plurality of PAA coated silver nanoparticles (“AgNPs@PAA”) are characterized as substantially mono-disperse nanoparticles having an average diameter of about 1.0 to 30 nm as indicated in ¶24 and 27 of Liu et al. where the average diameter of the AgNPs is ~2-5 nm. It has been held that a prima facie case of obviousness exists when the range disclosed in the prior art overlaps with the claimed range. See MPEP 2144.05(I) – OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 36, Liu et al. in view of Jesswein discloses the electrode of Claim 33, wherein the plurality of PAA coated silver nanoparticles (“AgNPs@PAA”) are characterized as substantially mono-disperse nanoparticles having an average diameter of about 1.0 to 10 nm as indicated in ¶24 and 27 of Liu et al. where the average diameter of the AgNPs is ~2-5 nm. It has been held that a prima facie case of obviousness exists when the range disclosed in the prior art overlaps with the claimed range. See MPEP 2144.05(I) – OVERLAPPING, APPROACHING, AND SIMILAR RANGES, AMOUNTS, AND PROPORTIONS.
Regarding Claim 37, Liu et al. in view of Jesswein discloses the electrode of Claim 33, wherein the plurality of PAA coated silver nanoparticles (“AgNPs@PAA”) are characterized as electrocatalysts toward hydrogen evolution in acidic media as indicated in ¶31 and 32 of Liu et al. where the catalytic HER performance is termed “excellent.” During the evaluation of HER activity, Liu et al. uses a 0.5 M H2SO4 electrolyte, which is acidic media (¶50 and 59).
Regarding Claim 38, Liu et al. in view of Jesswein discloses the electrode of Claim 33, but is silent on the altered crystal structure featuring a lower surface of atomic coordination number nor a lattice strain of about 0.5% to about 1% of the plurality of particles. The specification of the instant application indicates that in certain embodiments, the plurality of particles have a lower surface atomic coordination number on page 8 in ¶39 and that increasing the surface area of Ag results in more unsaturated coordination atoms on page 2 thereby improving the HER activity of said catalyst. Liu et al. discloses the electrode material Claim 33 which comprises PAA-coated silver nanoparticles which have increased surface area from the small particle size (2-5 nm diameter) and catalyze the HER reaction. Therefore, the electrode material of Claim 33 would inherently have an altered crystal structure featuring a lower surface of atomic coordination number as evidenced by, at least, the Applicant’s own disclosure (pg. 2 in ¶6 and pg. 8 ¶39). See MPEP 2112-III.
Regarding Claim 39, Liu et al. in view of Jesswein discloses the electrode of Claim 33, wherein the electrode material is characterized as a catalyst (toward hydrogen evolution reaction) as per ¶31 and 32 in Liu et el.
Regarding Claim 40, Liu et al. in view of Jesswein discloses the electrode of Claim 33, comprising a capping agent which is analogous to the aqueous polymer of Liu et al. (¶15 and 16). The aqueous polymer controls the size of the Ag particles, provides stability to the silver particles, coats the nanoparticles, and binds them into super particles (¶22, 24, 27, and 29).
Regarding Claim 41, Liu et al. in view of Jesswein discloses the electrode of Claim 33, but does not explicitly disclose the use of a carbon-based substrate (or electrode support). Nickel foam is a high surface area conductive material, but is susceptible to dissolution or leaching of nickel ions into the acidic electrolyte (e.g.: 0.5 M sulfuric acid). The presence of dissolved nickel ions can scavenge the electrons that are used to reduce protons to hydrogen gas during the hydrogen evolution reaction, thereby lowering the catalytic efficiency of the PAA-nano-silver electrode material. Conversely, glassy carbon supports (electrodes) are conductive and resistant to acid electrolytes. It would be obvious to one of ordinary skill in the art prior to the effective filing date of the claimed invention to substitute a glassy carbon electrode for the nickel foam support disclosed by Liu et al. in view of Jesswein with the reasonable expectation of increasing the catalytic efficiency of the PAA-AgNPs for hydrogen evolution reaction. See MPEP 2144.06(II) – Art Recognized Equivalence for the Same Purpose: Substituting Equivalent Known for the Same Purpose.
Response to Arguments
6. The examiner withdraws the objection to the specification in light of the applicant’s amendments as described on pg. 7-8 of the applicant’s response.
7. The examiner withdraws the objection under 35 USC § 112(b) of Claim 5 since said claim was cancelled by the applicant.
8. The applicant has cancelled all of the claims directed toward the electrode material (i.e.: Claims 1-19) so the examiner agrees the previous rejections are moot. The applicant has amended Claim 20 to now include the new limitation that the application of the electrode formulation occurs under a hydrogen atmosphere which was not previously presented. Therefore, the rejections from the FAOM has been withdrawn. However, upon further consideration, a new ground(s) of rejection is made in view of Liu et al. and Jesswein. The reasons for the new rejection of amended Claim 20, Claim 21, and new Claims 24-41 are explained in detail above.
Conclusion
9. 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.
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
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