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 .
Election/Restrictions
Applicant’s election without traverse of Group I, claims 1-15 in the reply filed on 8/13/2026 is acknowledged. Non-elected claims 16-19 have been cancelled.
Claim Rejections - 35 USC § 112
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 1-15 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.
Regarding claim 1, the term “defect-rich” in claim 1 is a relative term which renders the claim indefinite. The term “defect-rich” is not defined by the claim, the specification does not provide a standard for ascertaining the requisite degree, and one of ordinary skill in the art would not be reasonably apprised of the scope of the invention. It is noted that the claim indicates that the film has a vacancy density of up to 3.35 x 1014/cm2, however, that range also includes a value where there are no vacancies, such that it is not clear what the lower limit of vacancies is needed to provide a “defect-rich” monolayer. For the purposes of examination, having any range of vacancies within the claimed range is considered to meet the requirements of a “defect-rich” monolayer.
Claim 1 also recites the limitation "the MoS2 film" in line 3. There is insufficient antecedent basis for this limitation in the claim. For the purposes of examination, the claim is being interpreted as though the MoS2 film is the MoS2 monolayer.
Since none of the dependent claims remedy the clarity of claim 1, they are also rendered indefinite. Appropriate action is required without adding new matter.
Regarding claim 14, the claim recites the limitation "the target substrate" in line 3. There is insufficient antecedent basis for this limitation in the claim. The claim is dependent on claim 1, however, claim 8 provides antecedent basis for “the target substrate”. Therefore, it is unclear whether claim 14 is intended to depend on claim 8 as opposed to claim 1. For the purposes of examination, the claim is interpreted as dependent on claim 8. Appropriate action is required without adding new matter.
Claim Rejections - 35 USC § 102
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 the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
Claims 1-9, 14, and 15 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Man, “Salt-Induced High-Density Vacancy-Rich 2D MoS2 for Efficient Hydrogen Evolution” 2023 (provided on the IDS of 11/28/2023).
Regarding claim 1, Man teaches a method of producing a defect-rich molybdenum disulfide (MoS2) monolayer comprising vapor depositing the MoS2 monolayer on a growth substrate in the presence of potassium chloride (KCl), wherein the MoS2 film has a vacancy density up to 3.35 x 1014/cm2 (providing a salt-assisted CVD method for synthesizing ultrahigh-density vacancy-rich 2H-MoS2 monolayer with a controllable sulfur vacancy density of up to 3.35 x 1014 cm-2, abstract, where the growth substrate is pre-sprayed with a potassium chloride promoter prior to deposition, abstract and pg. 7, section 4). Therefore, the vacancy density is within the claimed range. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
Regarding claim 2, Man teaches the process of claim 1. They further teach the MoS2 monolayer is vapor deposited by,
(a) spraying a solution of the KCl on the growth substrate disposed in a reaction chamber (spraying KCl on the substrate, where the process is done in a furnace, pg. 7, section 4); and
(b) allowing a sulfur precursor to react with a molybdenum precursor at about 800 - 900°C in a flow of a carry gas for about 10-20 mins to deposit the MoS2 monolayer on the growth substrate (synthesizing the MoS2 at 840°C for 10 min while flowing Ar, pg. 7, section 4). Therefore, the temperature and time are within the claimed range. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
Regarding claims 3 and 4, Man teaches the process of claim 2. They further teach that the KCl solution has a concentration of 0.1, 0.5, 1.0 1.5, 2.0, 2.5, and 3.0 M (pg. 7, section 4), so as to be within the ranges of claims 3 and 4. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
Regarding claim 5, Man teaches the process of claim 2. They further teach using Ar as a carrier gas (pg. 7, section 4).
Regarding claims 6 and 7, Man teaches the process of claim 5. They further teach using Na2MoO4∙2H2O and sulfur powder as the molybdenum and sulfur sources (pg. 7, section 4).
Regarding claims 8 and 9, Man teaches the process of claim 1. They further teach transferring the MoS2 by spin-coating PMMA on the as-grown MoS2 at a speed of 3000 rpm for 60 s, detaching the PMMA/MoS2 film by emerging in 75°C KOH for ~1-15 mins, and transferring the film onto a device substrate or TEM grid (pg. 7, section 4). They teach that the PMMA could be washed with acetone, isopropanol, and ethanol respectively (pg. 7, section 4). Therefore, they provide the features of claim 8 and spin-coating for a time and speed meeting the requirements of claim 9. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
Regarding claims 14 and 15, Man teaches the process of claims 1 and 8. They further teach transferring the film onto a TEM grid or a device substrate such as one including Si (pg. 7, section 4 and Fig. 5).
Claim 1 is rejected under 35 U.S.C. 102(a)(1) as being anticipated by Li, US 2022/0288576 A1.
Regarding claim 1, Li teaches a method of producing a molybdenum disulfide (MoS2) monolayer comprising vapor depositing the MoS2 monolayer on a growth substrate in the presence of potassium chloride (KCI) (forming a metal chalcogenide by depositing a salt on a substrate and thermally co-depositing a metal oxide and a chalcogen onto the pre-deposited salt to form a patterned monolayer, 0057, where the salt is selected from a group including KCl, 0060, where the process is a CVD process so as to provide vapor deposition, 0084, and where the layer is formed on a substrate, 0084).
They teach using hydrogen together with argon or nitrogen as a carrier gas, where using different H2 concentrations controls the concentration of VS of the resulting MoS2 (0072). They teach that adjusting the Ar/H2 ratio allows tuning of VS concentrations, where it is typically ~6% and increases to ~10% and ~17% with an addition of 3.75% and 5% H2 (0084).
Therefore, they teach producing a MoS2 monolayer comprising vapor depositing the monolayer on a growth substrate in the presence of KCl, where the monolayer is considered to have a vacancy density within the claimed range since it is greater than zero. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
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.
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, 2, 5-9, 14, and 15 are rejected under 35 U.S.C. 103 as being unpatentable over Ly, “Catalyzed Kinetic Growth in Two-Dimensional MoS2”, 2020.
Regarding claims 1, 2, and 5-7, Ly teaches a method of producing a molybdenum disulfide (MoS2) monolayer comprising vapor depositing the MoS2 monolayer on a growth substrate in the presence of potassium chloride (KCI) (performing CVD growth of 2D MoS2 monolayers by using potassium chloride as a catalyst on a growth substrate, abstract, pg. 13131, Results and Discussion, and pg. S2, section 2).
They teach spraying a 0.05 M KCl solution on a plasma treated substrate surface in a plasma cleaner machine and then growing the MoS2 flakes on the treated substrate by CVD (pg. S2, section 2). They teach providing a boat with a Mo source such as Na2MoO4∙2H2O and a boat with sulfur powder in a tubular furnace and heating to a target temperature of 680-840°C, where the specific temperatures used include 680°C, 720°C, 760°C, 800°C, and 840°C (pg. S2, section 2 and Fig. S12). They teach holding at the temperature for 10 minutes (pg. S2, section 2). They teach using argon as a carrier gas at 200 sccm to transport sulfur vapor to the substrate location (pg. S2, section 2). They teach using substrates such as SiO2/Si and sapphire (pg. S2, section 2).
Therefore, they provide spraying a solution of KCl on the growth substrate disposed in a reaction chamber (plasma cleaner) and allowing a sulfur precursor to react with a molybdenum precursor at a temperature overlapping the claimed range in a flow of a carry gas (argon) for 10 minutes to deposit the MoS2 monolayer on the growth substrate, so as to provide the features of claims 2 and 5. They also provide a sulfur precursor (sulfur powder) and a molybdenum precursor (Na2MoO4∙2H2O) meeting the requirements of claims 6 and 7, where the flow rate of argon, the time for growth, and the temperature are within the range of claim 7.
While they do not teach the vacancy density, since they provide the process of claims 1, 2 and 5-7 for forming the MoS2 monolayer, the resulting material is also expected to have a vacancy density within the claimed range so as to provide a defect-rich MoS2 monolayer. According to MPEP 2112.01 I, “Where the claimed and prior art products are identical or substantially identical in structure or composition, or are produced by identical or substantially identical processes, a prima facie case of either anticipation or obviousness has been established. In re Best, 562 F.2d 1252, 1255, 195 USPQ 430, 433 (CCPA 1977)”. This is also supported by Fig. 3d of the instant specification which indicates that when using a KCl concentration of 0.05 M the defect density will be within the claimed range (note that the claimed range includes a vacancy density of 0).
Regarding claim 8, Ly suggests the process of claim 1. They further teach transferring the MoS2 by spin-coating a PMMA solution on the as-grown MoS2 layer to provide a PMMA/MoS2 film (pg. S2, section 2). They teach detaching the film from the fluorophlogopite mica by emerging in ultra-pure water, where for the SiO2/Si and sapphire substrates a KOH or NaOH solution was used, suggesting the substrates will also be emerged in KOH or NaOH (pg. S2, section). They teach using a TEM grid to scoop out the floating PMMA/MoS2 film so that the PMMA/MoS2 is attached totally on the TEM grid at room temperature and then introducing acetone evaporation to remove the PMMA film (pg. S2, section 2). Therefore, they provide the features of claim 8, where the acetone evaporation step of removing the PMMA is understood to be washing the PMMA/MoS2 target substrate with acetone solvent.
Regarding claim 9, Ly suggests the process of claim 8. They further teach spin-coating the PMMA solution on the substrate at 3000 rpm for 60 seconds (pg. S2, section 2), so as to meet the claimed requirements. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
Regarding claim 14, Ly suggests the process of claims 1 and 8. They further teach that the target substrate is a TEM grid and that the growth substrate is SiO2/Si (pg. S2, section 2).
Regarding claim 15, Ly suggests the process of claim 1, where the target substrate is a TEM grid. Since the selection of a semiconducting substrate is optional, Ly is considered to provide the features of claim 15.
Claims 3 and 4 are rejected under 35 U.S.C. 103 as being unpatentable over Ly as applied to claim 1 above, and further in view of Li, US 2022/0288576 A1.
Regarding claims 3 and 4, Ly suggests the process of claim 1, where they use a 0.05 M KCl solution (pg. S2, section 2).
They do not teach using a KCl concentration within the claimed range.
Li teaches catalyst compositions including metal chalcogenides and processes for producing such catalyst compositions (abstract). They teach processes for controlling and enhancing the electrocatalytic activity of metal chalcogenides and improved catalyst compositions (0029). They teach forming metal chalcogenides by CVD (0084). They teach pre-depositing a salt layer onto a substrate, where the salt is selected from a group including KCl (0057 and 0060). They teach that the MoS2 monolayer is deposited using a molybdenum precursor (MoO2) and a sulfur precursor (sulfur powder) (0059 and 0084). They teach heating from about 600°C to about 900°C (0071). They teach that the salt can be capable of providing a monolayer single crystal having large-sized domains and/or reducing strain of the growing monolayer films by passivating the edges of the domains (0060). They teach that the size and/or shape of the resulting MoS2 crystals can depend on one or more of the salt concentration deposited on the substrate, the weight ratio of starting material, the gas flow rate, and/or the processing times (0077).
From the teachings of Li, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have optimized the concentration of the salt in the solution that is sprayed to be within the claimed range because Li teaches that the concentration of salt deposited on the substrate can alter the size and/or shape of MoS2 crystals grown by CVD on the substrate such that by optimizing the concentration of KCl in the solution it will also be expected to optimize the concentration of salt on the substrate for controlling the growth of the MoS2 monolayer. According to MPEP 2144.05 II A, “Generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. “[W]here the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation.” In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955).
Claims 3 and 4 are alternatively rejected under 35 U.S.C. 103 as being unpatentable over Ly as applied to claim 1 above, and further in view of He, “Revisited Catalytic Hydrogen Evolution Reaction Mechanism of MoS2”, 2023.
Regarding claims 3 and 4, Ly suggests the process of claim 1, where they use a 0.05 M KCl solution (pg. S2, section 2).
They do not teach using a KCl concentration within the claimed range.
He teaches that defect engineering is an effective strategy to accelerate the catalytic hydrogen production of MoS2 (pg. 4, section 3). They teach that sulfur vacancies can be introduced into the MoS2 basal plane by controlling the reaction conditions during the MoS2 growth through a salt-assisted CVD method (pg. 4, section 3). They teach that the density of vacancies could be controlled by controlling the added amount of KCl during the CVD growth process (pg. 4, section 4). They teach that samples with abundant sulfur vacancies had the best catalytic hydrogen production performance and the lowest Tafel slope (pg. 5, section 4). They indicate that the lowest Tafel slope was provided for samples using a KCl concentration of 2.5 M (Fig. 3).
From the teachings of He, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have sprayed the substrate with a 2.5 M KCl solution because He teaches that such a concentration provides the best catalytic hydrogen production performance. Therefore, the concentration will be within the claimed range. According to MPEP 2131.03, “[W]hen, as by a recitation of ranges or otherwise, a claim covers several compositions, the claim is ‘anticipated’ if one of them is in the prior art.”
Claims 10-12 are rejected under 35 U.S.C. 103 as being unpatentable over Ly as applied to claim 1 above, and further in view of Liu, US 2020/0027921 A1 and Wang, “Effects of solvents and polymer on photoluminescence of transferred WS2 monolayers” 2019.
Regarding claims 10 and 11, Ly suggests the process of claim 1. They further teach emerging the substrates in water at 75°C for removing the fluorophologopite mica, but that KOH or NaOH is needed to detach from the SiO2/Si and sapphire substrates (pg. S2, section 2).
They do not teach the molarity or time for the removal.
Liu teaches a particle that includes a first sheet comprising a layer including a first material and a second sheet comprising a layer including a second material (abstract). They teach growing a MoS2 layer by CVD on a sapphire or SiO2 substrate (0231). They teach spin-coating a PMMA layer onto the surface of the MoS2/SiO2 surface and etching the SiO2 layer using 1 M KOH at 80°C (0234). They also teach using a 2M KOH solution to remove MoS2 from a SiO2 substrate at 80°C (0240).
Wang teaches a PMMA-assisted wet transfer process to transfer CVD-grown WS2 onto other substrates (abstract). They teach that WS2 monolayers grown on a 300 nm SiO2/Si substrate were covered with PMMA (pg. 052902-1-052902-2, section II, B). They teach that the PMMA/WS2/substrate layers were floated in a 30% KOH solution at room temperatures so that the KOH etched the SiO2 layer of the SiO2/Si substrate (pg. 052902-2, section II, B). They teach that the process separated the PMMA/WS2 layer from the substrate within 10 minutes depending on the concentration of the KOH solution (pg. 052902-2, section 2, B). They teach that the PMMA/WS2 layer was rinsed by DI water and then scooped onto another substrate (pg. 052902-2, section 2, B). They teach that the PMMA was removed using warm acetone followed by IPA rinsing and DI water rinsing (pg. 052902-2, section 2, B).
From the teachings of Ly, Liu, and Wang, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have etched the PMMA layer at a temperature of 75 or 80°C using an KOH solution having a molarity of 1 M using a time optimized to be within the claimed range because Ly teaches etching a substrate from the MoS2 layer using a temperature of 75°C, suggesting that such a temperature is suitable, Liu teaches removing SiO2 from a MoS2 by immersing in a 1M KOH solution at 80°C, and Wang teaches that time needed to detach a SiO2/Si substrate from a TMD layer using KOH is dependent on the concentration of the substrate such that by using a temperature of 75°C or 80°C and a molarity of 1 M it will be expected to successfully remove the substrate from the MoS2 layer. While 1 M is greater than 0.5 M and 80°C is higher than 76°C, according to 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) (Court held as proper a rejection of a claim directed to an alloy of "having 0.8% nickel, 0.3% molybdenum, up to 0.1% iron, balance titanium" as obvious over a reference disclosing alloys of 0.75% nickel, 0.25% molybdenum, balance titanium and 0.94% nickel, 0.31% molybdenum, balance titanium. "The proportions are so close that prima facie one skilled in the art would have expected them to have the same properties."). Therefore, a 1M KOH solution at 80°C is considered to be close enough to a 0.5 M solution at 75°C to provide similar results.
Alternatively, since Wang teaches that the time for removing the substrate depends on the concentration of the KOH, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have optimized the concentration of KOH and the time to be within the claimed range to enable removal of the substrate in an acceptable time frame. According to MPEP 2144.05 II A, “Generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. “[W]here the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation.” In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955). Therefore, the temperature is suggested to meet the claimed limitations or be close enough to expect similar results, the molarity is suggested to be optimized to be within the claimed range or close enough to expect similar results, and the time is suggested to be optimized to be within the claimed range.
Regarding claim 12, Ly in view of Liu and Wang suggest the process of claim 12. As discussed above for claim 8, Ly teaches removing the PMMA using acetone (pg. S2, section 2). Wang also teaches removing PMMA using acetone (pg. 052902-2, section 2, B). Liu also teaches removing PMMA by washing with acetone and ethanol (0321).
Claims 13 and 15 are rejected under 35 U.S.C. 103 as being unpatentable over Ly in view of Liu and Wang as applied to claim 1 above, and further in view of Neupane, “Simple Chemical Treatment to n-Dope Transition-Metal Dichalcogenides and Enhance the Optical and Electrical Characteristics”, 2017.
Regarding claim 13, Ly in view of Liu and Wang suggest the process of claim 12.
They do not teach washing with acetone, isopropanol, and ethanol in sequence.
Neupane teaches doping monolayer transition-metal dichalcogenides (abstract). They teach synthesizing MoS2 on SiO2/Si substrates by CVD (pg. 11955, Materials and Methods). They teach covering the CVD-grown films with PMMA and transferring them onto clean, thin glass substrates using the wet-transfer technique (pg. 11955, Materials and Methods). They teach etching the SiO2 using HF and transferring the film onto the glass substrate (pg. 11955, Materials and Methods). They teach removing PMMA residues by repeatedly cleaning with acetone, IPA, and ethanol (pg. 11955, Materials and Methods).
From the teachings of Neupane, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have removed the PMMA from the substrate by repeated washing with acetone, isopropanol, and ethanol because Neupane teaches that such a sequence is used for removing PMMA from a MoS2 film such that it will be expected to remove the PMMA as desired.
Regarding claim 15, Ly suggests the process of claim 14.
They do not teach transferring onto a glass substrate.
Neupane teaches doping monolayer transition-metal dichalcogenides (abstract). They teach synthesizing MoS2 on SiO2/Si substrates by CVD (pg. 11955, Materials and Methods). They teach covering the CVD-grown films with PMMA and transferring them onto clean, thin glass substrates using the wet-transfer technique (pg. 11955, Materials and Methods). They teach etching the SiO2 using HF and transferring the film onto the glass substrate (pg. 11955, Materials and Methods). They teach using the 1L-TMDs on the glass substrate for forming FET devices (pg. 11955, Materials and Methods).
From the teachings of Neupane, it would have been obvious to a person having ordinary skill in the art before the effective filing date of the claimed invention to have transferred the MoS2 monolayers onto a glass substrate because Neupane teaches that such a substrate is desirable for forming devices such as FET devices from MoS2 films.
Conclusion
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/CHRISTINA D MCCLURE/Examiner, Art Unit 1718
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