DETAILED ACTION
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 .
Claims 1-5, 7-8, 10-11, 14, 27-31 and 38-42 are pending.
Election/Restrictions
Applicant’s election without traverse of claims 1-5, 7-8, 10-11, 14 and 27-31 in the reply filed on 09/22/2025 is acknowledged.
Claim Objections
Claims 4, 10 and 27 are objected to because of the following informalities:
In claim 4, line 2, “chloride and” should read “chloride, and”.
In claim 10, line 4, “opacity;” should read “opacity; and”.
In claim 10, line 7, “transitions” should read “transitioning”.
In claim 27, line 11, “slurry;” should read “slurry; and”.
Appropriate correction is required.
Claim Rejections - 35 USC § 112(b)
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claims 27-31 are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention.
Claim 27 recites the limitation "the solvent" in lines 5, 6 and 9. There is insufficient antecedent basis for this limitation in the claim. The limitations of “a solvent” and “a first solvent” are previously introduced in lines 2 and 3 or the claim, respectively. It is therefore unclear which “solvent” is being referred to in the later recitations or if the “solvent” and “first solvent” are in fact the same element. For examination purposes, based on the similar independent claim 1, the “solvent” and “first solvent” will be interpreted as referring to the same element.
Claim 27 recites the limitation "the amount" in line 6. There is insufficient antecedent basis for this limitation in the claim. There is no previous mention of an “amount” in the claims.
Any claims dependent on the above claim(s) are rejected for their dependence.
Claim Rejections - 35 USC § 112(d)
The following is a quotation of 35 U.S.C. 112(d):
(d) REFERENCE IN DEPENDENT FORMS.—Subject to subsection (e), a claim in dependent form shall contain a reference to a claim previously set forth and then specify a further limitation of the subject matter claimed. A claim in dependent form shall be construed to incorporate by reference all the limitations of the claim to which it refers.
The following is a quotation of pre-AIA 35 U.S.C. 112, fourth paragraph:
Subject to the following paragraph [i.e., the fifth paragraph of pre-AIA 35 U.S.C. 112], a claim in dependent form shall contain a reference to a claim previously set forth and then specify a further limitation of the subject matter claimed. A claim in dependent form shall be construed to incorporate by reference all the limitations of the claim to which it refers.
Claim 11 is rejected under 35 U.S.C. 112(d) or pre-AIA 35 U.S.C. 112, 4th paragraph, as being of improper dependent form for failing to further limit the subject matter of the claim upon which it depends, or for failing to include all the limitations of the claim upon which it depends. Claim 11 recites the limitation of the nanoparticle assembly comprising the platinum nanoparticles that are combined via the one or more grain boundaries. This fails to further limit claim 1 which recites in lines 6-8 that the platinum nanoparticles have assembles into a nanoparticle assembly in which they are connected via one or more grain-boundaries. Applicant may cancel the claim(s), amend the claim(s) to place the claim(s) in proper dependent form, rewrite the claim(s) in independent form, or present a sufficient showing that the dependent claim(s) complies with the statutory requirements.
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.
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.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claims 1, 7-8, 10-11, 14 and 40-41 are rejected under 35 U.S.C. 103 as being unpatentable over Plyasova et al. (“Electrodeposited platinum revisited: Tuning nanostructure via the deposition potential”, Electrochem Acta, 2006) in view of Stolarczyk et al. (“Nanoparticle Clusters: Assembly and Control Over Internal Order, Current Capabilities, and Future Potential”, Adv. Mater., 2016), and further in view of Prieve et al. (“2-D assembly of colloidal particles on a planar electrode”, Curr. Opin. Colloid Interface Sci., 2010) and Hu et al. (“Rapid Synthesis of Cubic Pt Nanoparticles and Their Use for the Preparation of Pt Nanoagglomerates”, J. Nanosci. Nanotechnol., 2006); claim 40 evidenced by Aabdin et al. (“Bonding Pathways of Gold Nanocrystals in Solution”, Nano Lett, 2014).
Regarding claim 1, Plyasova teaches a method (see e.g. Page 4476, Col. 1, bottom paragraph, method of producing nanostructured Pt) comprising:
receiving, within a receptacle of an electrolysis reactor, a solvent that contains platinum (see e.g. Page 4476, Col. 2, 2nd paragraph, lines 2-3, and 3rd paragraph lines 1-2, H2PtCl6 solution in electrochemical cell);
activating a first electrode and a second electrode of the electrolysis reactor to apply a voltage to the solvent (see e.g. Page 4476, Col. 2, 1st-2nd paragraphs, and 3rd paragraph, lines 1-4, four electrode cell with working electrode and counter electrode used to apply deposition potential of 0.025-0.55 V);
and assembling individual nanoparticles into a nanoparticle assembly, the platinum nanoparticles of the nanoparticle assembly connected via one or more grain boundaries (see e.g. Abstract and Page 4480, bottom paragraph, lines 8-9, Pt nanostructures, i.e. assemblies, formed by nm-sized crystallites interconnected via grain boundaries).
Plyasova does not teach the platinum being in the form of nanoparticles suspended within the solvent by a ligand compound, instead teaching it being in the form of a Pt precursor (see e.g. Page 4476, Col. 2, 2nd paragraph, lines 2-3, and 3rd paragraph lines 1-2, H2PtCl6 solution). Plyasova does however teach the interplay of primary and secondary nucleation contributing to the formation of the interconnected nanoparticle assembly (see e.g. Page 4480, bottom paragraph, lines 8-11, and Page 4479, connecting paragraph of Cols. 1-2, lines 11-16).
Stolarczyk teaches a method of forming nanoparticle assemblies (see e.g. Abstract) comprising a two-step process in which a stable suspension of nanoparticles suspended by ligands is initially formed, followed by an independent assembly process of the nanoparticles by application of an external stimulus (see e.g. Scheme 1 and Page 5400, Col. 2, lines 23-27), this two-step colloidal assembly having the advantages over in situ NP synthesis/cluster assembly of producing stable and high quality nanoparticle building blocks as well as producing ordered/controlled nanoparticle assemblies by engineering the NP-NP interaction potentials (see e.g. Page 5400, Col. 2, bottom paragraph, lines 1-18).
Prieve teaches a method of forming an assembly from colloidal particles by applying an electrical voltage between electrodes in a bulk solution containing the particles (see e.g. Abstract, Page 162, Col. 1, lines 13-16, and Page 172, Col. 2, bottom paragraph, lines 1-6)
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of Plyasova to comprise a two step colloidal assembly process in which a suspension of the platinum nanoparticles with ligands is initially formed and added to the electrolysis reactor and then undergo independent assembly via application of an external stimuli such as the electrolysis voltage as taught by Stolarczyk and Prieve to allow production of stable and high quality nanoparticle building blocks and ordered/controlled nanoparticle assemblies by engineering the NP-NP interaction potentials
Modified Plyasova does not explicitly teach determining, based at least on a state of the solvent, that the individual platinum nanoparticles have assembled into the nanoparticle assembly.
Hu teaches a method of synthesizing Pt nanoparticles and nanoagglomerates, i.e. nanoparticle assemblies (see e.g. Abstract), in which complete formation of the nanoagglomerates from a solution including nanoparticles was confirmed by a change in solution color (see e.g. Page 2057, Col. 1, Section 2.3, lines 6-15, Page 2059, bottom paragraph, lines 5-12, and Page 2060, paragraph starting “To gain…”).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of modified Plyasova to comprise determining that the platinum nanoparticles have assembled upon detecting a change in the color of the solution/solvent, as taught by Hu as a suitable means of confirming the complete formation of agglomerated Pt nanoparticle assemblies. MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 7, Plyasova as modified by Stolarczyk teaches the ligand compound being a capping agent reducing the occurrence of individual nanoparticles of the platinum nanoparticles from combining with each other within the solvent (see e.g. Stolarczyk Scheme 1, stable suspension of individual nanoparticles capped by ligands which repel each other; Page 5402, Col. 1, bottom paragraph, lines 1-7).
Regarding claim 8, Plyasova as modified by Stolarczyk and Prieve teaches the voltage being determined to remove the ligand compound from the platinum nanoparticles and destabilize the platinum nanoparticles; and the voltage causing the platinum nanoparticles to collide to form the nanoparticle assembly after removal of the ligand compound (see e.g. Stolarczyk Scheme 1, Page 5402, connecting paragraph of Cols. 1-2, lines 6-12, and Page 5406, Col. 1, bottom paragraph, lines 4-6, ligand removal from individual nanoparticles and aggregation of said nanoparticles into clusters/assemblies via application of external stimulus; see e.g. Prieve Abstract, externally applied electrical voltage causing colloidal particles to aggregate).
Regarding claim 10, Plyasova as modified by Hu teaches determining that the platinum nanoparticles have been assembled into the nanoparticle assembly comprising: determining a first state of the solvent, the first state characterized by a first color and first opacity; and determining that the solvent has transitioned from the first state to a second state, the second state characterized by a second color and second opacity and the solvent transitioning from the first state to the second state due to the platinum nanoparticles being assembled (see e.g. Hu Page 2057, Col. 1, Section 2.3, lines 6-15, Page 2059, bottom paragraph, lines 5-12, and Page 2060, paragraph starting “To gain…”, solution including Pt seeds turns from opaque creamy solution to homogeneous blackish brown, indicating formation of the Pt nanoagglomerates).
Regarding claim 11, modified Plyasova teaches the nanoparticle assembly comprising the platinum particles that are combined via the one or more grain boundaries (see e.g. Plyasova Abstract and Page 4480, bottom paragraph, lines 8-9, Pt nanostructures, i.e. assemblies, formed by nm-sized crystallites interconnected via grain boundaries).
Regarding claim 14, modified Plyasova teaches extracting the nanoparticle assembly from the solvent and cleaning the nanoparticle assembly (see e.g. Plyasova Page 4478, Col. 2, 2nd paragraph, lines 1-3, 3rd paragraph, lines 1-4, 4th paragraph lines 1-4, and 5th paragraph, deposited Pt removed from 4 electrode cell with deposition solution and moved to 3 electrode cell with H2SO4 for CV characterization, and additionally being repeatedly cleaned before further XRD and SEM studies).
Regarding claim 40, modified Plyasova teaches the one or more grain-boundaries comprising a highly-disordered grain-boundary and a low-disorder grain-boundary (see e.g. Plyasova Page 4477, Col. 2, lines 14-17, Page 4481, Col. 2, lines 3-10, and Page 4484, Col. 2, lines 9-12 and 16-18, highly defective grain boundaries along with less defective crystal coalescence; which are evidenced by Aabdin to be respectively indicative of an alignment angles of greater than 15° and less than 15°, see e.g. Aabdin Abstract, defect-free bonding below 15° and defect-mediated above 15°, equivalent to highly-disordered and low disorder as described in paragraph 0062 of the instant specification).
Regarding claim 41, Plyasova as modified by Stolarczyk and Prieve teaches individual platinum nanoparticles having a first diameter within the solvent; and the platinum nanoparticles of the nanoparticle assembly having a second diameter, the first diameter being substantially equal to the second diameter (see e.g. Stolarczyk Page 5400, Col. 2, bottom paragraph, lines 2-6 and 12-13, the nanoparticle building blocks forming the assembly are made to be stable, e.g. in size, remaining essentially the same after assembly; see e.g. Prieve Fig. 1, particles aggregated by electric field remaining essentially the same size as when individual).
Claims 2-4 are rejected under 35 U.S.C. 103 as being unpatentable over Plyasova, Stolarczyk, Prieve and Hu, as applied to claim 1 above, and further in view of Towsley (U.S. Patent No. 4,053,371) and Ustarroz et al. (“A Generalized Electrochemical Aggregative Growth Mechanism”, J. Am. Chem. Soc., 2013).
Regarding claim 2, modified Plyasova teaches all the elements of the method of claim 1 as stated above. Plyasova further teaches the first electrode being formed from a first platinum foil and being a positive electrode for providing the voltage (see e.g. Plyasova Page 4478, Col. 2, 2nd paragraph, lines 3-4, and 3rd paragraph, lines 1-4, Pt foil counter electrode performing oxidation, i.e. as a positive electrode, as the working electrode performs reduction of the Pt ions to Pt(0)), the second electrode being formed from a second foil and being a negative electrode for providing the voltage (see e.g. Plyasova Page 4478, Col. 2, 1st paragraph, lines 1-3, and 3rd paragraph, lines 1-4, gold foil working electrode performing reduction, i.e. as a negative electrode, of Pt ions to Pt(0)); and the electrolysis reactor utilizing a third electrode configured as a reference electrode for the voltage (see e.g. Plyasova Page 4478, Col. 2, 2nd paragraph, lines 4-5).
Modified Plyasova does not teach the second foil being platinum, instead teaching it being gold (see e.g. Plyasova Page 4478, Col. 2, 1st paragraph, lines 1-3).
Towsley teaches a method electrolytically depositing metal (see e.g. Abstract) in which anode and cathode materials employed may include Au or Pt, optionally with the metal to be deposited serving as the anode or cathode (see e.g. Col. 3, lines 8-12).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the foil of the second electrode of modified Plyasova to be platinum, the same as the deposited metal, instead of gold as taught by Towsley as an alternate suitable electrode material for electrolytic deposition of a metal. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious.
Modified Plyasova does not teach the third electrode being formed from silver and silver chloride, instead teaching it being a reversible hydrogen electrode or mercury sulfate electrode (see e.g. Plyasova Page 4478, Col. 2, 2nd paragraph, lines 4-7).
Ustarroz teaches a method of electrochemical aggregative deposition of Pt nanostructures (see e.g. Abstract and Fig. 1) which utilizes an Ag/AgCl reference electrode (see e.g. Page 11552, Col. 1, under “Experimental Section”, lines 4-8).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the reference electrode of modified Plyasova to be formed from silver and silver chloride as taught by Ustarroz as an alternate suitable reference electrode for use in the electrochemical deposition method. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious. Further, MPEP § 2144.07 states “The selection of a known material based on its suitability for its intended use supported a prima facie obviousness determination in Sinclair & Carroll Co. v. Interchemical Corp., 325 U.S. 327, 65 USPQ 297 (1945)”.
Regarding claim 3, Plyasova as modified by Stolarczyk teaches the receptacle further comprising a base solution that the solvent, the platinum nanoparticles and the ligand compound are added to (see e.g. Plyasova Page 4476, Col. 2, 2nd paragraph, lines 1-3, and 3rd paragraph, lines 1-5, 0.01 M HCl solution containing the platinum precursor; see e.g. Stolarczyk Scheme 1, nanoparticles and ligand in suspension).
Regarding claim 4, modified Plyasova teaches the base solution being an aqueous solution that is saturated with a chloride, and the first electrode, the second electrode, and the third electrode are at least partially submerged in the base solution (see e.g. Plyasova Page 4476, Col. 2, 2nd paragraph, lines 1-5, and 3rd paragraph, lines 1-5, working, counter and reference electrodes in cell with 0.01M aqueous HCl solution).
Plyasova, as modified above, does not explicitly teach the chloride being potassium chloride, instead teaching it being HCl (see e.g. Plyasova Page 4476, Col. 2, 3rd paragraph, lines 1-5).
Ustarroz further teaches a KCl solution being used with the platinum precursor for electrochemical deposition (see e.g. Ustarroz Page 11552, Col. 1, under “Experimental Section”, lines 1-4).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the chloride solution of modified Plyasova to be a potassium chloride solution as taught by Ustarroz as a suitable base solution for electrochemical Pt deposition. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious.
Claims 5 and 38 are rejected under 35 U.S.C. 103 as being unpatentable over Plyasova, Stolarczyk, Prieve and Hu, as applied to claim 1 above, and further in view of Mazzotta et al. (“Bare Platinum Nanoparticles Deposited on Glassy Carbon Electrodes for Electrocatalytic Detection of Hydrogen Peroxide”, ACS Appl. Nano Mater., July 2021).
Regarding claim 5, modified Plyasova teaches all the elements of the method of claim 1 as stated above. Plyasova as modified by Stolarczyk further teaches receiving the platinum nanoparticles further comprising receiving a platinum ion precursor that is provided to the solvent (see e.g. Plyasova Page 4476, Col. 2, 3rd paragraph, lines 1-5, H2PtCl6 in solution); and receiving a ligand precursor that is provided to the solvent (see e.g. Stolarczyk Scheme 1, free ligands initially in solution). Modified Plyasova does not explicitly teach receiving a reducing agent that is provided to the solvent, the reducing agent causing the platinum nanoparticles to form within the solvent and the ligand precursor to combine with the platinum nanoparticles as the ligand compound. Stolarczyk does however teach the nanoparticle precursors and ligand precursors transforming into the nanoparticles combined with the ligand compound to form a stable suspension (see e.g. Stolarczyk Scheme 1 and Page 5400, Col. 2, lines 25-26).
Mazzotta teaches a method of preparing Pt nanoparticles stabilized by citrate molecules (see e.g. Abstract and Page 7651, Col. 2, bottom paragraph, lines 2-6), comprising adding a hexachloroplatinic acid (H2PtCl6) solution to water, followed by adding sodium citrate and a quick addition of sodium borohydride, i.e. a reducing agent, to form the Pt nanoparticles with attached citrate molecules (see e.g. Page 7652, Col. 1, under “Experimental Section”, lines 4-7 and 23-30, and Page 7654, Col. 1, lines 6-10).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of modified Plyasova to comprise receiving the platinum ion precursor, ligand precursor and a reducing agent in the solvent, the reducing agent causing the formation of the platinum nanoparticles and combination with the ligand compound as taught by Mazzotta as a suitable specific method for providing a stable suspension of Pt nanoparticles with attached ligands. MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 38, Plyasova as modified by Mazzotta teaches the platinum ion precursor being hydrogen hexachloroplatinate (IV) hexahydrate (see e.g. Mazzotta Page 7652, Col. 1, under “Experimental Section”, lines 4-5 and 23-24, chloroplatinic acid (H2PtCl6) hexahydrate; Plyasova Page 4476, Col. 2, 3rd paragraph, lines 1-5, H2PtCl6); the ligand precursor being sodium citrate tribasic dihydrate (see e.g. Mazzotta Page 7652, Col. 1, under “Experimental Section”, line 6); and the reducing agent being sodium borohydride (see e.g. Mazzotta Page 7652, Col. 1, under “Experimental Section”, line 7).
Claim 39 is rejected under 35 U.S.C. 103 as being unpatentable over Plyasova, Stolarczyk, Prieve and Hu, as applied to claim 8 above, and further in view of Rosa-Ortiz et al. (“Study the impact of CuSO4 and H2SO4 concentrations on lateral growth of hydrogen evolution assisted copper electroplating”, J Appl Electrochem, 2019).
Regarding claim 39, modified Plyasova teaches all the elements of the method of claim 8 as stated above. Modified Plyasova does not explicitly teach the voltage electrolyzing the solvent such that one or more gaseous compounds are output by the solvent, the one or more gaseous compounds forming bubbles that agitate the platinum nanoparticles and cause collisions between the platinum nanoparticles. Prieve does however teach that fluid flow contributes to aggregation at the electrodes (see e.g. Prieve Page 165, Col. 2, under “Mechanisms for aggregation”, lines 1-9). Stolarczyk similarly teaches that perturbation of the nanoparticle suspension leads to the formation of the nanoparticle assembly (see e.g. Stolarczyk Page 5420, Col. 2, lines 1-5).
Rosa-Ortiz teaches a metal electrodeposition method in which the voltage was set high enough for water electrolysis and hydrogen evolution (see e.g. Abstract), the release of hydrogen bubbles producing fluid convection that assists the motion of metal ions beyond the limited diffusion rate (see e.g. Page 1209, Col. 1, bottom 3 lines, and Col. 2, lines 1-2).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of modified Plyasova to comprise setting the voltage high enough for water electrolysis and hydrogen evolution as taught by Rosa-Ortiz to produce fluid convection by release of hydrogen bubbles that can assist the motion, i.e. agitation/perturbation, of the platinum nanoparticles and thereby facilitate collision as desired by Prieve and Stolarczyk.
Claim 42 is rejected under 35 U.S.C. 103 as being unpatentable over Plyasova, Stolarczyk, Prieve and Hu, as applied to claim 14 above, and further in view of Reetz et al. (U.S. Patent No. 5,620,584).
Regarding claim 42, modified Plyasova teaches all the elements of the method of claim 14 as stated above. Modified Plyasova does not explicitly teach the extracting comprising at least one of: removing the solvent from the nanoparticle assembly via pipette; filtering the nanoparticle assembly from the solvent; or evaporating the solvent.
Reetz teaches a method of electrochemical preparation of metal nanostructures (see e.g. Col. 2, lines 27-29), wherein after the electrochemical preparation, the prepared nanostructure may be collected by a process including filtering from and/or drying/evaporation of the solvent used in the preparation (see e.g. Col. 11, lines 51-55, Col. 12, lines 11-19).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the extracting of modified Plyasova to comprise a process including filtering and/or evaporation of solvent from the nanoparticle assembly as taught by Reetz as a particular suitable method of collecting metal nanostructures obtained by an electrochemical process. MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Claims 27, 29 and 31 are rejected under 35 U.S.C. 103 as being unpatentable over Plyasova in view of Stolarczyk, and further in view of Prieve, Hu, Matsumiya et al. (“Nano-structured thin-film Pt catalyst for thermoelectric hydrogen gas sensor”, Sensors and Actuators B, 2003) and Altmann et al. (“Novel catalytic gas sensors based on functionalized nanoparticle layers”, Sensors and Actuators B, 2012).
Regarding claim 27, Plyasova teaches a method (see e.g. Page 4476, Col. 1, bottom paragraph, method of producing nanostructured Pt) comprising:
receiving, within a receptacle of an electrolysis reactor, a solvent that contains platinum (see e.g. Page 4476, Col. 2, 2nd paragraph, lines 2-3, and 3rd paragraph lines 1-2, H2PtCl6 solution in electrochemical cell);
activating, at a first time, a first electrode and a second electrode of the electrolysis reactor to apply a voltage to the solvent (see e.g. Page 4476, Col. 2, 1st-2nd paragraphs, and 3rd paragraph, lines 1-4, four electrode cell with working electrode and counter electrode used to apply deposition potential of 0.025-0.55 V);
assembling platinum nanoparticles into a nanoparticle assembly, the platinum nanoparticles of the nanoparticle assembly connected via one or more grain boundaries (see e.g. Abstract and Page 4480, bottom paragraph, lines 8-9, Pt nanostructures, i.e. assemblies, formed by nm-sized crystallites interconnected via grain boundaries); and
extracting the nanoparticle assembly from the solvent (see e.g. Page 4478, Col. 2, 2nd paragraph, lines 1-3, 3rd paragraph, lines 1-4, and 4th paragraph lines 1-4, deposited Pt removed from 4 electrode cell with deposition solution and moved to 3 electrode cell with H2SO4 for CV characterization).
Plyasova does not teach the platinum being in the form of nanoparticles that are suspended within a first solvent and are stabilized by a ligand compound, instead teaching it being in the form of a Pt precursor (see e.g. Page 4476, Col. 2, 2nd paragraph, lines 2-3, and 3rd paragraph lines 1-2, H2PtCl6 solution). Plyasova does however teach the interplay of primary and secondary nucleation contributing to the formation of the interconnected nanoparticle assembly (see e.g. Page 4480, bottom paragraph, lines 8-11, and Page 4479, connecting paragraph of Cols. 1-2, lines 11-16).
Stolarczyk teaches a method of forming nanoparticle assemblies (see e.g. Abstract) comprising a two-step process in which a stable suspension of nanoparticles suspended by ligands is initially formed, followed by an independent assembly process of the nanoparticles by application of an external stimulus (see e.g. Scheme 1 and Page 5400, Col. 2, lines 23-27), this two-step colloidal assembly having the advantages over in situ NP synthesis/cluster assembly of producing stable and high quality nanoparticle building blocks as well as producing ordered/controlled nanoparticle assemblies by engineering the NP-NP interaction potentials (see e.g. Page 5400, Col. 2, bottom paragraph, lines 1-18).
Prieve teaches a method of forming an assembly from colloidal particles by applying an electrical voltage between electrodes in a bulk solution containing the particles (see e.g. Abstract, Page 162, Col. 1, lines 13-16, and Page 172, Col. 2, bottom paragraph, lines 1-6).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of Plyasova to comprise a two-step colloidal assembly process in which a suspension of the platinum nanoparticles with ligands is initially formed and added to the electrolysis reactor and then undergo independent assembly via application of an external stimuli such as the electrolysis voltage as taught by Stolarczyk and Prieve to allow production of stable and high quality nanoparticle building blocks and ordered/controlled nanoparticle assemblies by engineering the NP-NP interaction potentials
Modified Plyasova does not explicitly teach determining, based at least on the solvent, that the platinum nanoparticles have been assembled to form the nanoparticle assembly.
Hu teaches a method of synthesizing Pt nanoparticles and nanoagglomerates, i.e. nanoparticle assemblies (see e.g. Abstract), in which complete formation of the nanoagglomerates from a solution including nanoparticles was confirmed by a change in solution color (see e.g. Page 2057, Col. 1, Section 2.3, lines 6-15, Page 2059, bottom paragraph, lines 5-12, and Page 2060, paragraph starting “To gain…”).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of modified Plyasova to comprise determining that the platinum nanoparticles have assembled upon detecting a change in the color of the solution/solvent, as taught by Hu as a suitable means of confirming the complete formation of agglomerated Pt nanoparticle assemblies. MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Modified Plyasova does not teach the extracted nanoparticle assembly being purified to obtain a nanoparticle assembly powder, mixing the nanoparticle assembly powder with a second solvent to form a nanoparticle slurry, and forming a hydrogen sensor from a temperature sensor and the nanoparticle slurry, wherein the temperature sensor is coated with the nanoparticle assembly to create the hydrogen sensor. Plyasova does however teach the platinum nanoparticle assembly with interconnected grains being used as a catalyst (see e.g. Plyasova Abstract and Page 4478, Col. 1, lines 2-5).
Matsumiya teaches a hydrogen gas sensor with prominent selectivity (see e.g. Abstract) comprising a thermoelectric oxide film, i.e. temperature sensor, with a platinum catalyst film on part of its surface (see e.g. Abstract and Page 309, Col. 1, lines 16-18, and Col. 2, lines 7-10), the platinum catalyst comprising a nanostructured Pt film with clusters of nano-sized Pt grains (see e.g. Page 311, Col. 1, lines 5-8).
Altmann teaches a thermal hydrogen gas sensor (see e.g. Abstract) comprising a thermoelectric sensing element with Pt nanoparticles deposited on one side as a catalytic layer (see e.g. Figs. 1-2 and Page 146, under “Materials and methods”, lines 1-7 and 23-25), wherein, for deposition onto the sensor, the prepared Pt nanoparticles are separated from the solution in which they prepared and washed, i.e. purified, thereby creating a powder which is then redissolved in a more volatile solvent to form a second solution, i.e. slurry, which is used for deposition onto the sensor (see e.g. Page 147, Col. 1, lines 5-15 and 34-39).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of modified Plyasova to comprise the platinum nanoparticle assembly being incorporated into a hydrogen sensor by purification into a powder and redissolving into a more volatile solvent to form a second solution/slurry for coating a thermoelectric film, i.e. temperature sensor, as taught by Matsumiya and Altmann as a particular use of the nanoparticle assembly as a catalyst that benefits from its interconnected grains and a suitable method of incorporating the nanoparticle assembly prepared in solution onto said sensor.
MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 29, Plyasova as modified by Altmann teaches the nanoparticle slurry being a suspension of the nanoparticle assembly within the second solvent (see e.g. Altmann Page 147, Col. 1, lines 13-14, solution of particles in acetone, i.e. forming suspension).
Regarding claim 31, Plyasova as modified by Altmann teaches the second solvent being evaporated from the nanoparticle slurry that coats the temperature sensor to deposit the nanoparticle assembly on the temperature sensor (see e.g. Altmann Page 147, Col. 1, paragraph starting “Due to…”, lines 8-10, nanoparticle layer remaining on sensor surface after solvent evaporation).
Claim 28 is rejected under 35 U.S.C. 103 as being unpatentable over Plyasova, Stolarczyk, Prieve, Hu, Matsumiya and Altmann, as applied to claim 27 above, and further in view of Lee et al. (U.S. 2011/0017597).
Regarding claim 28, modified Plyasova teaches all the elements of method of claim 27 as stated above. Plyasova as modified by Altmann further teaches the nanoparticle assembly powder being dissolved in the second solvent (see e.g. Altmann Page 147, Col. 1, lines 13-14, particles redissolved in acetone). Modified Plyasova does not teach the second solvent being an alcohol, instead exemplifying it being acetone or toluene (see e.g. Altmann Page 147, Col. 1, lines 13-14 and 27-29), which are organic solvents, but does generally teach it being a volatile solvent (see e.g. Altmann Page 147, Col. 1, lines 7-9).
Lee teaches a method of fabricating a sensor for detecting hydrogen gas (see e.g. Abstract) wherein a platinum powder as catalyst particles is dispersed in an organic solvent such as isopropyl alcohol, this dispersion then being loaded onto a surface and the organic solvent vaporized to lead the platinum on the surface (see e.g. Paragraphs 0026-0027 and 0034).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the second solvent of modified Plyasova to instead comprise isopropyl alcohol as an alternate suitable volatile organic solvent for dispersion and then evaporation in coating of platinum catalyst particles on a sensor surface. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious. MPEP § 2144.07 states “The selection of a known material based on its suitability for its intended use supported a prima facie obviousness determination in Sinclair & Carroll Co. v. Interchemical Corp., 325 U.S. 327, 65 USPQ 297 (1945)”.
Claim 30 is rejected under 35 U.S.C. 103 as being unpatentable over Plyasova, Stolarczyk, Prieve, Hu, Matsumiya and Altmann, as applied to claim 27 above, and further in view of Molter et al. (U.S. 2018/0372701).
Regarding claim 30, modified Plyasova teaches all the elements of method of claim 27 as stated above. Modified Plyasova does not teach forming the hydrogen sensor further comprising submerging the temperature sensor within the nanoparticle slurry to coat the temperature sensor with the nanoparticle assembly, instead teaching the nanoparticle slurry being stamped in the temperature sensor (see e.g. Altmann Page 147, Col. 1, paragraph starting “Due to…”, lines 1-6).
Molter teaches a hydrogen monitoring/sensing system (see e.g. Abstract) in which catalytic materials such as platinum may be in the form of particles dispersed in an ink and deposited onto electrode by a method such as dipping, i.e. of the electrodes into said ink (see e.g. Paragraph 0030).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the method of modified Plyasova to comprise dipping, i.e. submerging, the temperature sensor into the nanoparticle slurry as taught by Molter as an alternate suitable means of depositing catalytic particles onto a surface of a hydrogen sensor. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious.
Conclusion
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/M.S.J./Examiner, Art Unit 1795
/LUAN V VAN/Supervisory Patent Examiner, Art Unit 1795