DETAILED ACTION
Response to Amendment
This is a final office action in response to a communication filed on June 5, 2026. Claims 1-10 are pending in the application.
Status of Objections and Rejections
All rejections under 35 U.S.C. §103 are maintained.
Claim Rejections - 35 USC § 103
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
Claim(s) 1-10 is/are rejected under 35 U.S.C. 103 as being unpatentable over Wang (X. Wang, Silicon/Hematite Core/Shell Nanowire Array Decorated with Gold Nanoparticles for Unbiased Solar Water Oxidation, Nano Letters, 2014 (14), pp. 18-23; supplemental information was attached) in view of Zhang (L. Zhang, MoS2-wrapped silicon nanowires for photoelectrochemical water reduction, Nano Research 2015 (8), pp. 281-287), and further in view of Toe (C.Y. Toe, Recent advances and the design criteria of metal sulfide photocathodes and photoanodes for photoelectrocatalysis, J. Mater. Chem. A, 2021(9), pp. 20277-20319).
Regarding claim 1, Wang teaches a photoelectrocatalyst ([Abstract]: three-dimensional (3D) silicon/hematite core/shell nanowire arrays decorated with gold nanoparticles (AuNPs) for sunlight-driven solar water splitting), comprising:
a substrate, formed of a semiconductor material, the substrate having an upper surface (Fig. 1(a): Silicon; the silicon substrate having a top surface), the semiconductor material having a first conductive type (Fig. 1(b): p-Si; Fig. 1(a), 2(a): indicating the substrate and the p-SiNW has the same semiconductor material, Si);
a plurality of nanowires (Fig. 1(a): SiNW), formed of the semiconductor material (Fig. 1(b): the SiNW array comprising p-Si) and formed on the upper surface of the substrate (Fig. 1(a): the nanowire array formed on the top surface of the Si substrate);
a plurality of metal nanoparticles (Fig. 1(a): gold nanoparticles), being formed on the plurality of nanowires (Supplemental, Fig. S3(a): inner configuration), each nanowire thereon existing a few of the plurality of metal nanoparticles (Fig. 1(a); Fig. S3(a): each nanowire having a few of the plurality of the gold nanoparticles formed thereon).
Wang does not teach a transition metal compound film, formed to overlap the plurality of nanowires and the plurality of metal nanoparticles, the transition metal compound film being formed of a transition metal sulfide, the transition metal compound film has a second conductive type different from the first conductive type.
However, Zhang teaches molybdenum disulfide (MoS2) wrapped semiconductor nanowires (NWs) as a well-defined MoS2/TiO2/Si coaxial NW heterostructure, which yield photocurrent density up to 15 mA/cm2 with good stability (Zhang, [Abstract]). Although Zhang teaches a photocathode, Toe teaches metal sulfides have tunability of p-type and n-type behaviors and have been extensively employed as both photocathodes and/or photoanodes (Toe, [Abstract]). N-type materials are used as photoanodes for oxidation reaction, and p-type materials are made into photocathodes for reduction reaction (p. 20279, col. 2, para. 1). For example, photoanode has been discovered using TiO2, followed by Fe2O3 (p. 20291, col. 1, para. 2), and recently using metal sulfide, e.g., MoS2, due to their suitable band structure, excellent charge kinetics, tailorable architecture, chemical composition and optical properties; particularly, most of the binary and ternary sulfide materials possess n-type properties (p. 20291, col. 1, para. 3). Thus, MoS2 is commonly fabricated as n-type material to be used as photoanode sulfide materials (p. 20291, col. 2, para. 2) by deposition on the TiO2 nanotube arrays (e.g., p. 20293, Fig. 14(a), (e)). The formation of a bulk-heterojunction between MoS2 and WS2 nanosheets has increased the rate of water oxidation and improved the PEC performance by up to 10 fold (p. 20295, col. 2, para. 1).
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 Wang by substituting hematite with MoS2 nanosheet wrapping the semiconductor nanowires as taught by Zhang and Toe because Zhang teaches a suitable heterostructured photoelectrocatalyst (Zhang [Abstract]: molybdenum disulfide (MoS2) wrapped semiconductor nanowires (NWs) as a well-defined MoS2/TiO2/Si coaxial NW heterostructure) and the formation of a bulk-heterojunction used as n-type sulfide materials for the photoanode would increase the rate of water oxidation and improved the PEC performance by up to 10 fold (Toe, p. 20295, col. 2, para. 1). As a result, the substitution would necessarily result in the transition metal compound film formed to overlap the plurality of nanowires and the plurality of metal nanoparticles (see Wang Supplement, Fig. S3(a): Hematite overlaps both SiNW and gold nanoparticles). Also, the n-type sulfide materials are used as photoanodes for oxidation reaction (Toe, p. 20279, col. 2, para. 1), and thus the transition metal compound film has a n-type that is different from the first conductive type (Wang, Fig. 1(b): p-Si substrate and NW).
Regarding claim 2, Wang teaches wherein the plurality of metal nanoparticles are formed of gold (Fig. 1(a), 2(a); Fig. S3(a): gold nanoparticles).
Regarding claim 3, Wang in view of Zhang and Toe teaches the first conductive type is a p-type (Wang, Fig. 1(b): p-Si substrate and NW), the second conductive is an n-type (Toe, p. 20291, col. 2, para. 2: photoanode material, e.g., MoS2 and WS2, are commonly fabricated as n-type materials).
Regarding claim 4, Wang, Zhang, and Toe disclose all limitations of 2.
Wang does not disclose the first conductive type is an n-type, the second conductive is a p-type or the transition metal compound film is formed of Ag2S.
However, Zhang teaches the MoS2/TiO2/Si coaxial NW heterostructure is designed to be a photocathode ([Abstract]). In order to achieve a positive photovoltage, a heavily doped n+ emitter layer was diffused into the surface region of Si NWs using arsenic (As) as an n-type dopant to form a MoS2/TiO2/n+p-Si NW coaxial heterostructure (p. 285, col. 1, para. 2), making the first conductive type a n-type. Further, Toe teaches n-type materials are used as photoanodes for oxidation reaction, and p-type materials are made into photocathodes for reduction reaction, and thus a p-type semiconductor will be coupled with an n-type semiconductor, forming a p-n junction to optimize the charge separation efficiency (p. 20279, col. 2, para. 1). Toe further discloses the most attractive features of metal sulfide materials is their tailorable semiconducting type, i.e., n- or p-type (p. 20279, col. 1, para. 2), and Ag2S is an appropriate material for photoelectrode material (bridging sentence of pp. 20292-20293). Thus, to design a photocathode and using n-type Si NWs of the combined Wang and Zhang would necessarily require the outer transition metal compound film, e.g., Ag2S, to be p-type as suggested by Toe and result in a heterostructure.
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 Wang, Toe, and Zhang by switching the p-type Si NWs into n-type (Wang, p. 19, col. 1, last para.) and utilizing p-type photoabsorbers (e.g., Ag2S) as the transition metal compound film to be a photocathode because n-type materials are used as photoanodes for oxidation reaction and p-type materials are made into photocathodes for reduction reaction (Toe, p. 20279, col. 2, para. 1). Here, the claimed limitations are obvious because all 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 yielded nothing more than predictable results. MPEP 2143(I)(A). Further, there are only two types of the semiconductor conductivity, so choosing from a finite number of identified, predictable solutions, with a reasonable expectation of success is prima facie obvious. MPEP 2141(III)(E).
Regarding claim 5, Wang, Zhang, and Toe disclose all limitations of claim 2. Wang further discloses wherein a height of each nanowire ranges from 0.5 µm to 15 µm (Fig. 3(a): the height is about 5 µm).
Wang, Zhang, and Toe do not disclose a diameter of each nanowire ranges from 10 nm to 100 nm.
However, Wang disclose the SiNWs have diameter of 30-200 nm (p. 20, col. 2, para. 1), which overlaps the claimed range.
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 Wang, Zhang, and Toe by adjusting the diameter of the nanowire within the claimed range because they are suitable nanowire dimension for loading photoelectrocatalyst. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990). MPEP 2144.05(I). Similarly, a prima facie case of obviousness exists where the claimed ranges or amounts do not overlap with the prior art but are merely close. Titanium Metals Corp. of America v. Banner, 778 F.2d 775, 783, 227 USPQ 773, 779 (Fed. Cir. 1985). MPEP 2144.05(I).
Wang, Zhang, and Toe do not disclose a particle size of each metal nanoparticle ranges from 5nm to 50 nm.
However, Wang disclose a particle size of AuNPs about 4 nm (Fig. 3(c)).
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 Wang, Zhang, and Toe do by adjusting the AuNP size within the claimed range because they are suitable dimension of AuNPs to be loaded on the SiNWs. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990). MPEP 2144.05(I). Similarly, a prima facie case of obviousness exists where the claimed ranges or amounts do not overlap with the prior art but are merely close. Titanium Metals Corp. of America v. Banner, 778 F.2d 775, 783, 227 USPQ 773, 779 (Fed. Cir. 1985). MPEP 2144.05(I).
Regarding claim 6, Wang teaches a method of fabricating a photoelectrocatalyst ([Abstract]: three-dimensional (3D) silicon/hematite core/shell nanowire arrays decorated with gold nanoparticles (AuNPs) for sunlight-driven solar water splitting), comprising the steps of:
preparing a substrate, wherein the substrate is formed of a semiconductor material (Fig. 1(a): Silicon substrate) and has a first conductive type (Fig. 1(b): p-Si; Fig. 1(a), 2(a): indicating the substrate and the p-SiNW has the same semiconductor material, Si);
partially etching the upper surface of the substrate downwards (p. 20, col. 2, para. 1: SiNWs arrays were prepared on Si wafers by means of the metal-catalyzed electroless etching (MCEE) method) to form a plurality of nanowires (Fig. 1(a): SiNW);
depositing a plurality of metal nanoparticles (Fig. 1(a): gold nanoparticles) on the plurality of nanowires (Supplemental, Fig. S3(a): inner configuration), wherein each nanowire thereon exists a few of the plurality of metal nanoparticles (Fig. 1(a); Fig. S3(a): each nanowire having a few of the plurality of the gold nanoparticles formed thereon).
Wang does not teach forming a transition metal compound film to overlap the plurality of nanowires and the plurality of metal nanoparticles, wherein the transition metal compound film is formed of a transition metal sulfide, the transition metal compound film has a second conductive type different from the first conductive type.
However, Zhang teaches molybdenum disulfide (MoS2) wrapped semiconductor nanowires (NWs) as a well-defined MoS2/TiO2/Si coaxial NW heterostructure, which yield photocurrent density up to 15 mA/cm2 with good stability (Zhang, [Abstract]). Although Zhang teaches a photocathode, Toe teaches metal sulfides have tunability of p-type and n-type behaviors and have been extensively employed as both photocathodes and/or photoanodes (Toe, [Abstract]). N-type materials are used as photoanodes for oxidation reaction, and p-type materials are made into photocathodes for reduction reaction (p. 20279, col. 2, para. 1). For example, photoanode has been discovered using TiO2, followed by Fe2O3 (p. 20291, col. 1, para. 2), and recently using metal sulfide, e.g., MoS2, due to their suitable band structure, excellent charge kinetics, tailorable architecture, chemical composition and optical properties; particularly, most of the binary and ternary sulfide materials possess n-type properties (p. 20291, col. 1, para. 3). Thus, MoS2 is commonly fabricated as n-type material to be used as photoanode sulfide materials (p. 20291, col. 2, para. 2) by deposition on the TiO2 nanotube arrays (e.g., p. 20293, Fig. 14(a), (e)). The formation of a bulk-heterojunction between MoS2 and WS2 nanosheets has increased the rate of water oxidation and improved the PEC performance by up to 10 fold (p. 20295, col. 2, para. 1).
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 Wang by substituting hematite with MoS2 nanosheet wrapping the semiconductor nanowires as taught by Zhang and Toe because Zhang teaches a suitable heterostructured photoelectrocatalyst (Zhang [Abstract]: molybdenum disulfide (MoS2) wrapped semiconductor nanowires (NWs) as a well-defined MoS2/TiO2/Si coaxial NW heterostructure) and the formation of a bulk-heterojunction using n-type MoS2 sulfide materials as the photoanode would increase the rate of water oxidation and improved the PEC performance by up to 10 fold (Toe, p. 20295, col. 2, para. 1). As a result, the substitution would necessarily result in the transition metal compound film formed to overlap the plurality of nanowires and the plurality of metal nanoparticles (see Wang Supplement, Fig. S3(a): Hematite overlaps both SiNW and gold nanoparticles). Also, the n-type materials are used as photoanodes for oxidation reaction (Toe, p. 20279, col. 2, para. 1), and thus the transition metal compound film has a n-type that is different from the first conductive type (Wang, Fig. 1(b): p-Si substrate and NW).
Regarding claim 7, Wang teaches wherein the plurality of metal nanoparticles are formed of gold (Fig. 1(a), 2(a); Fig. S3(a): gold nanoparticles).
Regarding claim 8, Wang in view of Zhang and Toe teaches wherein the first conductive type is a p-type (Wang, Fig. 1(b): p-Si substrate and NW), the second conductive is an n-type, the transition metal compound film is formed of MoS2 (Toe, p. 20291, col. 2, para. 2: photoanode material, e.g., MoS2 and WS2, are commonly fabricated as n-type materials).
Regarding claim 9, Wang, Zhang, and Toe disclose all limitations of 7.
Wang does not disclose the first conductive type is an n-type, the second conductive is a p-type or the transition metal compound film is formed of Ag2S.
However, Zhang teaches the MoS2/TiO2/Si coaxial NW heterostructure is designed to be a photocathode ([Abstract]). In order to achieve a positive photovoltage, a heavily doped n+ emitter layer was diffused into the surface region of Si NWs using arsenic (As) as an n-type dopant to form a MoS2/TiO2/n+p-Si NW coaxial heterostructure (p. 285, col. 1, para. 2), making the first conductive type a n-type. Further, Toe teaches n-type materials are used as photoanodes for oxidation reaction, and p-type materials are made into photocathodes for reduction reaction, and thus a p-type semiconductor will be coupled with an n-type semiconductor, forming a p-n junction to optimize the charge separation efficiency (p. 20279, col. 2, para. 1). Toe further discloses the most attractive features of metal sulfide materials is their tailorable semiconducting type, i.e., n- or p-type (p. 20279, col. 1, para. 2), and Ag2S is an appropriate material for photoelectrode material (bridging sentence of pp. 20292-20293). Thus, to design a photocathode and using n-type Si NWs of the combined Wang and Zhang would necessarily require the outer transition metal compound film, e.g., Ag2S, to be p-type as suggested by Toe and result in a heterostructure.
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 Wang, Toe, and Zhang by switching the p-type Si NWs into n-type (Wang, p. 19, col. 1, last para.) and utilizing p-type photoabsorbers (e.g., Ag2S) as the transition metal compound film as photocathode because n-type materials are used as photoanodes for oxidation reaction and p-type materials are made into photocathodes for reduction reaction (Toe, p. 20279, col. 2, para. 1). Here, the claimed limitations are obvious because all 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 yielded nothing more than predictable results. MPEP 2143(I)(A). Further, there are only two types of the semiconductor conductivity, so choosing from a finite number of identified, predictable solutions, with a reasonable expectation of success is prima facie obvious. MPEP 2141(III)(E).
Regarding claim 10, Wang, Zhang, and Toe disclose all limitations of claim 7. Wang further discloses wherein a height of each nanowire ranges from 0.5 µm to 15 µm (Fig. 3(a): the height is about 5 µm).
Wang, Zhang, and Toe do not disclose a diameter of each nanowire ranges from 10 nm to 100 nm.
However, Wang disclose the SiNWs have diameter of 30-200 nm (p. 20, col. 2, para. 1), which overlaps the claimed range.
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 Wang, Zhang, and Toe by adjusting the diameter of the nanowire within the claimed range because they are suitable nanowire dimension for loading photoelectrocatalyst. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990). MPEP 2144.05(I). Similarly, a prima facie case of obviousness exists where the claimed ranges or amounts do not overlap with the prior art but are merely close. Titanium Metals Corp. of America v. Banner, 778 F.2d 775, 783, 227 USPQ 773, 779 (Fed. Cir. 1985). MPEP 2144.05(I).
Wang, Zhang, and Toe do not disclose a particle size of each metal nanoparticle ranges from 5nm to 50 nm.
However, Wang disclose a particle size of AuNPs about 4 nm (Fig. 3(c)).
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 Wang, Zhang, and Toe do by adjusting the AuNP size within the claimed range because they are suitable dimension of AuNPs to be loaded on the SiNWs. In the case where the claimed ranges "overlap or lie inside ranges disclosed by the prior art" a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990). MPEP 2144.05(I). Similarly, a prima facie case of obviousness exists where the claimed ranges or amounts do not overlap with the prior art but are merely close. Titanium Metals Corp. of America v. Banner, 778 F.2d 775, 783, 227 USPQ 773, 779 (Fed. Cir. 1985). MPEP 2144.05(I).
Response to Arguments
Applicant’s arguments with respect to claims 1-10 have been considered but are unpersuasive.
Applicant argues the substitution of hematite in Wang with MoS2 from Zhang lacks adequate motivation and would destroy the operability of Wang’s device (Response, p. 3, section 2) because Wang is directed to a photoanode for water oxidation and Zhang is directed to a photocathode for water reduction (p. 4, para. 2). Examiner agrees that Wang is directed to photoanode for oxidation and Zhang is directed to photocathode for reduction. However, the prior art, Toe, is relied on to teach n-type materials are used as photoanodes for oxidation reaction and p-type materials are made into photocathodes for reduction reaction (Toe, p. 20279, col. 2, para. 1), and the most attractive features of metal sulfide material is their tailorable semiconducting type (i.e., n- or p-type) (Toe, p. 20279, col. 1, para. 2). Thus, metal sulfide materials (e.g., MoS2) can be used as either a photocathode (p. 20281, col. 1, section 3) or as a photoanode (p. 20291, col. 1, section 4). MoS2 is commonly fabricated as n-type materials to be used as photoanode (p. 20291, col. 2, para. 2). The instant rejection is rewritten to clarify that Zhang is relied on to teach the photoelectrode configuration, i.e., each nanowire is wrapped with MoS2 (p. 282, col. 2, para. 3; Fig. 1(a)-(b): the MoS2 as a transition metal compound film on the nanowires), and Toe is relied on to teach the opposite conductive types of the substrate/nanowires and the transition metal compound film.
Applicant argues Zhang teaches a TiO2 interlayer between the Si NWs and MoS2 and the claimed invention does not utilize any TiO2 or other interlayer (bridging para. of pp. 4-5). This argument is unpersuasive. First, claim 1 recites a heterostructured photoelectrocatalyst using an open transition term “comprising” which does not exclude other components besides all recited components. Second, Zhang’s TiO2 interlayer corresponding to the hematite of Wang, which would be substituted by the transition metal compound.
Applicant argues the film must encapsulate/wrap both the NWs and the AuNPs (p. 5, para. 2). Examiner refers to Wang Supplemental Fig. S3(a), the inner configuration, in which the hematite encapsulate both silicon NWs and gold nanoparticles (please see the supplemental information after Wang publication, Supplemental, p. 5). Thus, the substitution of hematite with MoS2 would necessarily result in the transition metal compound encapsulating both NWs and AuNPs.
In response to Applicant’s argument regarding claims 3 and 8 (pp. 6-8), Examiner notes that the rejection relies on Wang’s teaching of p-type substrate and NWs (Wang, Fig. 1) and Toe’s teaching of n-type materials used as photoanode sulfide materials, e.g., MoS2 (Toe, p. 20291, col. 2, para. 2). In response to Applicant’s argument regarding claims 4 and 9 (pp. 8-9), Examiner notes that the rejection relies on Wang’s teaching of n-type substrate and NWs (Wang, p. 19, col. 1, last para.) and Toe’s teaching of p-type photoabsorbers used as photocathode sulfide materials, e.g., Cu2S and SnS (Toe, p. 20281, col. 2, para. 2). Also Examiner notes that Toe explicitly discloses n-type materials are used as photoanodes for oxidation reaction, and p-type materials are made into photocathodes for reduction reaction, and thus a p-type semiconductor will be coupled with an n-type semiconductor, forming a p-n junction to optimize the charge separation efficiency (p. 20279, col. 2, para. 1). Toe also teaches that the most attractive features of metal sulfide materials is their tailorable semiconducting type, i.e., n- or p-type (p. 20279, col. 1, para. 2).
Applicant argues the recited nanowire diameter range (10 nm to 100 nm) is critical by citing Fig. 9-10 and ¶66 that discloses a preferred diameter of about 50 nm (p. 10, para. 2). This argument is unpersuasive. Wang’s teaching on the diameter range, 30-200 nm, overlaps the recited range from 10 nm to 100 nm. Applicant fails to provide evident supporting the criticality of the recited range (from 10 nm to 100 nm) among the disclosed range (from 20 to 200 nm) in the prior art. In response to Applicant’s argument regarding the nanoparticle size range (pp. 10-11), Examiner notes that even if the claimed ranges or amounts do not overlap with the prior art but when they are merely close, a prima facie case of obviousness exists. Titanium Metals Corp. of America v. Banner, 778 F.2d 775, 783, 227 USPQ 773, 779 (Fed. Cir. 1985). MPEP 2144.05(I). Applicant fails to provide evident supporting any surprising or unexpected results caused by gold nanoparticles in the claimed 5-50 nm range rather than that using 4 nm gold nanoparticles in the prior art.
Conclusion
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 extension fee 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.
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/C. SUN/Primary Examiner, Art Unit 1795
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