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 .
Claim Interpretation
Claim 15 requires generating the plasma through “low-pressure” reactant gas discharge. “Low-pressure” is being interpreted as being any pressure below atmospheric.
Status of the Claims
Claims 1-18 are pending and rejected. Claims 19 and 20 are withdrawn. Claim 1 is amended.
Claim Rejections - 35 USC § 112
The following is a quotation of the first paragraph of 35 U.S.C. 112(a):
(a) IN GENERAL.—The specification shall contain a written description of the invention, and of the manner and process of making and using it, in such full, clear, concise, and exact terms as to enable any person skilled in the art to which it pertains, or with which it is most nearly connected, to make and use the same, and shall set forth the best mode contemplated by the inventor or joint inventor of carrying out the invention.
The following is a quotation of the first paragraph of pre-AIA 35 U.S.C. 112:
The specification shall contain a written description of the invention, and of the manner and process of making and using it, in such full, clear, concise, and exact terms as to enable any person skilled in the art to which it pertains, or with which it is most nearly connected, to make and use the same, and shall set forth the best mode contemplated by the inventor of carrying out his invention.
Claims 1-18 are rejected under 35 U.S.C. 112(a) or 35 U.S.C. 112 (pre-AIA ), first paragraph, as failing to comply with the written description requirement. The claim(s) contains subject matter which was not described in the specification in such a way as to reasonably convey to one skilled in the relevant art that the inventor or a joint inventor, or for applications subject to pre-AIA 35 U.S.C. 112, the inventor(s), at the time the application was filed, had possession of the claimed invention.
Regarding claim 1, the claim has been amended to indicate that the growing, the harvesting, and the collecting of the graphene are all performed under a shared atmosphere within the deposition chamber, however, the claim does not have support for a “shared atmosphere”. Applicant’s arguments dated 12/31/2025 indicate that a shared atmosphere provides the same pressure, temperature, and gaseous constitution, however, the specification does not have support for this feature. While the specification at page 7, lines 12-25 indicates that the cleaning is done at the same conditions, i.e., temperature and pressure, as during subsequent deposition of the primary carbon layer and growth of graphene, there is no indication that the entire chamber has the same gaseous constitution. The process is a PECVD process, where the figures depict the plasma generator as being located near the gas distribution region as in Fig. 2-4. For the entire process to have the same gaseous constitution, the plasma would also have to be throughout the chamber. Since the dependent claims do not remedy the new matter of claim 1, they are also considered to include new matter.
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 1-18 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, claim 1 has been amended to indicate that the process is done under a “shared atmosphere”, however, it is unclear what constitutes a “shared atmosphere”. Applicant’s arguments dated 12/31/2025 indicate that a shared atmosphere provides the same pressure, temperature, and gaseous constitution, however, the specification does not have support for this feature. Further, the earth is under a shared atmosphere, but there are different temperature, pressures, and gases in the shared atmosphere. Similarly, a vacuum chamber can be supplied with a gaseous mixture under a single pressure but can have different temperatures within the chamber and the gases can mix differently within the chamber. For the purposes of examination, a “shared atmosphere” is interpreted as a single chamber where processes are done without requiring the use of gas curtains as was suggested by He. 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.
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, 2, and 7-18 are rejected under 35 U.S.C. 103 as being unpatentable over Boyd, US 2014/0044885 A1 in view of Na, US 2013/0233480 A1, Zaretski, US 2015/0371848 A1, Cooper, US 2012/0251432 A1, and Park, US 2016/0130150 A1.
Regarding claims 1, 9, and 10, Boyd teaches a method for continuous production of graphene by means of an apparatus (a method for growing high quality large area graphene, 0053, where an apparatus for the process is a continuous roll-to-roll system so as to provide continuous production of large area graphene, 0061 and Fig. 8), the method comprising:
providing a clean surface on a rotatable substrate (where the surface of the substrate is subjected to a hydrogen plasma with trace amount of methane or a carbon source to remove copper oxide while depositing graphene, 0053 and 0057, indicating that the surface will be cleaned during deposition to provide a clean surface, where the process can be done using a roll-to-roll system, 0061 and Fig. 8, indicating that the substrate is rotatable since it can be wound on a roll);
depositing a primary carbon layer onto the surface of the rotatable substrate from a carbon-containing gas via plasma-enhanced chemical vapor deposition (depositing graphene on to the copper surface using a plasma of hydrogen and a carbon source gas, 0053-0055, 0057-0058, and Fig. 6, such that a primary carbon layer, i.e., graphene, is deposited on the substrate by PECVD since it is a plasma vapor deposition of gaseous sources that will chemically react to form graphene); and
continuously growing graphene on the primary carbon layer via plasma-enhanced chemical vapor deposition by addition of the carbon-containing gas to a deposition chamber (where the process provides graphene growth, where single layers or multi-layer graphene can be provided, 0038, 0057, and 0058, where the carbon source is provided to the chamber during deposition, Fig. 6 and Fig. 8, and where the process is a continuous roll-to-roll process, 0061 and Fig. 8, such that graphene will be continuously grown on the primary carbon layer, i.e., the initial graphene layer when forming multiple layers by PECVD with continuous addition of the carbon-containing gas to the chamber).
They do not teach continuously harvesting the graphene grown on the primary carbon layer while leaving the primary carbon layer on the rotatable substrate.
Na teaches a method for transferring graphene that includes a graphene synthesizing operation comprising forming at least one layer of graphene on at least one surface of a catalyst metal film, a substrate film attaching operation comprising contacting an adhesive first surface of the substrate film to the at least one layer of graphene and compressing the catalyst metal film and the substrate film by using a first roller, and a substrate film separating operation comprising separating the substrate film from the catalyst metal film such that the at least one layer for graphene is separated from the catalyst metal film together with the substrate film (abstract, Fig. 1, and Fig. 5). They teach forming graphene on the catalyst surface by CVD, where the catalyst is a metal such as copper (0020 and 0038). They teach that the substrate film is treated to be adhesive (0023). They teach that the substrate film is unwound from a winding reel and is pressed against the surface of the graphene film on the catalyst (0025). They each that the film separating operation is performed where the adhesive force between the substrate film and the graphene is greater than that between the catalyst metal film and the graphene so that the substrate film and the graphene layer are separated from the catalyst (0031, Fig. 1, and Fig. 5). They teach that when forming multi-layered graphene, since a bonding force between layers of the multi-layered graphene is weak, when the substrate film is separated from the catalyst metal film, only layer 20a of graphene adheres to the adhesive first surface of the substrate film and is separated from the catalyst surface such that a graphene layer 20b remains on the catalyst surface (0043 and Fig. 8). They teach that a second separating operation can be performed to separate the remaining graphene layer 20b (0046 and Fig. 5). They teach that the graphene transfer method is simplified compared to prior techniques, the speed is increased, and damage to the graphene cause during a graphene transfer operation is effectively reduced (0010).
Zaretski teaches processes for transferring high quality large-area graphene layers to a flexible substrate based on preferential adhesion of certain thin metallic films to graphene followed by lamination of the metallized graphene layers to a flexible target substrate in a process that is compatible with roll-to-roll manufacturing, providing an environmentally benign and scalable process of transferring graphene to flexible substrate (abstract). They teach that the metal foil (e.g., copper foil or nickel foil) substrate is indefinitely reusable and the method is substantially greener than current processes using corrosive iron(III) chloride to etch the metal (0005). They teach manufacturing a graphene layer on a substrate comprising providing a graphene layer disposed on a first substrate, applying a metal layer to the graphene layer to form a metallized graphene layer, removing (e.g., peeling, exfoliating) the metallized graphene layer from the first substrate, and applying the metallized graphene layer to a second substrate (0006). They teach that the graphene layer can be a monolayer or comprise two or more layers (0008). They teach that growth of the graphene layer on the metal foil can be accomplished by PECVD (0027). They teach that the first substrate can be a metal foil such as copper or nickel (0029). After metallizing the graphene layer, they teach exfoliating the metallized graphene layer by peeling using van Der Waals bonds, electrostatic force, magnetic force, or pressure differential (0031). They teach that following the removal of the metal/graphene bilayer films, the metal substrate (e.g., the copper substrate) is reusable for CVD without further treatment (0040). They teach cleaning the copper foil in solvent prior to growth and electropolishing (0052-0053). They teach synthesizing graphene using CVD, metallizing with e-beam evaporation, and removing the graphene layer (0054-0057). They teach determining the reusability of the copper foil in the MAE process, where the quality of the graphene increased after successive cycles of growth (0068). They teach that after MAE, a small amount of graphene remains on the copper foil, indicating that small patches of a second graphene layer form beneath the first layer during graphene growth on copper by CVD (0069). They teach that the residual graphene grains serve as “seed grains” for the subsequent cycle of graphene growth, where it has been shown that best quality CVD graphene on copper is obtained by “pre-seeding” graphene grains on the copper surface prior to synthesis (0069).
From the teachings of Na and Zaretski, 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 modified the process of Boyd to have integrated the transfer operation of Na into the continuous deposition process so as to continuously harvest and collect the graphene while leaving a primary layer of graphene on the surface because Na provides a graphene transfer operation that is simplified compared to prior techniques, the speed is increased, and damage to the graphene cause during a graphene transfer operation is effectively reduced, where the process results in a remaining layer of graphene on the catalyst surface and Zaretski teaches that providing a graphene seeding layer resulting from residual graphene remaining on the substrate after peeling graphene from a catalyst surface improves the quality of the graphene deposited in subsequent cycles such that it will be expected to provide the benefits of the transfer process of Na while also improving subsequently deposited graphene quality on the catalyst surface due to the remaining primary layer acting as graphene seeds. Therefore, in the process of Boyd in view of Na and Zaretski, the graphene will be continuously harvested by being transferred to another substrate while leaving the primary carbon layer, i.e., residual seeding layer remaining on the rotatable foil, and collecting the graphene removed from the primary carbon layer by the film transfer process. Further, 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 cleaned the substrate using a solvent as in the process of Zaretski because they teach that such a cleaning step is desirable prior to depositing a graphene layer. Therefore, Boyd in view of Na and Zaretski suggest cleaning the substrate by a step prior to depositing and a step during depositing.
They do not teach that the rotatable substrate comprises an endless surface.
Cooper teaches a scaled method for producing carbon nanotubes by depositing onto a continuously moving substrate having a catalyst to initiate and maintain the growth of the CNTS and a carbon-bearing precursor (abstract). They teach that the process is continuous or semi-continuous where a catalyst is deposited to initiate and maintain the growth of carbon nanotubes and a carbon-breading precursor is provided to grow nanotubes inside of a CVD reactor (0009-0012). They teach that the moveable substrate may comprise metals (0014). They teach depositing the catalyst using CVD or PECVD (0016). They teach that the catalyst can be iron, cobalt, nickel, platinum, lead, palladium, copper, gold or any combination or alloy thereof (0019). They teach that the process describes large-scale production methods for producing nanostructure material (0056). They teach a continuous method may employ a rotating belt that permits treating of the deposition substrate before depositing carbon nanotubes thereon, where treating may include a plasma etch or chemical clean to clean the surface prior to depositing a catalyst support (0086 and Fig. 2). They teach that the system includes an exfoliation system, such as a blade, to remove the surface grown nanotubes from the substrate (0086 and Fig. 2). They teach that a roll-to-roll system may be used as an alternative to the belt (0087 and Fig. 3-4). Therefore, Cooper teaches that an endless belt is an alternative to a roll-to-roll system, where the system can include an electrode for plasma cleaning, a metal deposition system, a carbon material deposition system, and a material removal system.
From the teachings of Cooper, 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 modified the process of Boyd in view of Na and Zaretski to have used a continuous belt system for the deposition of graphene because Cooper teaches that an endless belt is an alternative to a roll to roll system, where the system can include an electrode for plasma cleaning, a carbon material deposition system, and a material removal system, where after removal of the graphene layer from the substrate of Boyd in view of Na and Zaretski, the surface is primed for further deposition of graphene (due to the graphene seed layer) and Zaretski teaches that the substrate is indefinitely reusable such that it will be expected to provide a continuous deposition process for graphene to as to improve the efficiency of the process. Therefore, in the process of Boyd in view of Na, Zaretski, and Cooper, the surface of the rotatable substrate will comprise an endless surface. Further, since Na provides a roll-to-roll process and Cooper indicates that the endless belt is an alternative to an endless roll, the process is expected to also be compatible with an endless belt process.
They do not teach that the growing, the harvesting, and the collecting of the graphene are all performed under a shared atmosphere within the deposition chamber.
Boyd further teaches performing the deposition process at a pressure of less than or equal to 500 mTorr (0054), so as to overlap the ranges of claims 9 and 10, therefore, the process is done under vacuum.
Cooper depicts depositing the catalyst on the substrate, growing carbon nanotubes, and harvesting/collecting the nanotubes in the same chamber (Fig. 2).
Park teaches a method of manufacturing graphene that includes preparing a support member, disposing a carbon layer on the support member, disposing a catalyst layer on the carbon layer, forming graphene on the catalyst layer, attaching a carrier to the graphene and forming a graphene-forming-structure, separating the support member from the graphene-forming structure, and removing the catalyst layer (abstract). They teach using an apparatus that includes a support member supplier, a carbon layer-forming unit, a catalyst layer-forming unit, a graphene-forming unit, a carrier supplier, a stacking device, a support member collector, a catalyst layer remover, and a carrier collector (0018 and Fig. 1). They teach that the reactor for forming graphene is a PECVD reactor using hydrocarbon gases (0028-0029). They teach that a carrier is a film tape that is pressed against the graphene layer (0035-0037). They teach a support member collector that separates the support member from the graphene-forming structure (0038). They teach that the graphene-manufacturing apparatus may include a vacuum chamber and a vacuum unit for allowing an entire process to be performed under a vacuum state (0046).
From the teachings of Park and Cooper, 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 provided the growing, harvesting and collecting all in a single vacuum chamber such that the processes share the same atmosphere because Park teaches that a roll-to-roll transfer process can occur in a vacuum chamber with a PECVD reactor used to deposit graphene and Cooper teaches growing and harvesting/collecting carbon nanotubes the same chamber such that it will be expected to provide the operations in a single vacuum chamber while also maintaining the cleanliness of the process.
Regarding claim 2, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Boyd further teaches that a fan or other cooling device was applied to the region of the processing tube in which the RF plasma is formed, reducing the temperature of the processing environment to reduce the temperature of the outside of the processing chamber to 90°C or other comparable temperatures (0056). They teach that the invention refers to room temperature growth of the graphene film, but that the temperature is not limited to growth at 24°C, but can include other comparable temperatures (0056). They teach that room temperature, is intended to include processing environments in which there is no external heating of the substrate other than the heat that can be generated as a result of the RF plasma process (0056). They teach that cooling can be used to remove a portion or all of the heat generated during the RF plasma process (0056). Therefore, when a portion of the heat is removed at least a portion of the apparatus will be heated from the RF plasma process and when the temperature outside of the processing chamber is reduced to 90°C or other comparable temperature, at least a portion of the apparatus will be heated so as to provide such a temperature outside of the chamber.
Regarding claim 7, Boyd in view of Na, Zaretski, Cooper, Park suggest the process of claim 1. Boyd teaches using carbon-containing gasses such as methane, ethane, acetylene, ethylene, propane, propylene, etc. (0055).
Regarding claim 8, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Boyd further teaches using hydrogen as a carrier gas where other gases such as nitrogen, argon, and the like can be used in addition to hydrogen (0055).
Regarding claims 11 and 12, Boyd in view of Na, Zaretski, Cooper, Park suggest the process of claim 1. Boyd teaches that the process may refer to room temperature growth of graphene, but the temperature is not limited to growth at 24°C and can include other comparable temperatures (0056). They teach cooling so that the temperature outside of the processing chamber is 90°C (0056). They teach reducing the temperature of the processing environment, for example, to temperatures less than room temperature (0056). Therefore, the continuous production of graphene is considered to be performed at a temperature within or overlapping the range of claims 11 and 12 since it is indicated as being done at room temperature or below. 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.” According to MPEP 2144.05, “in the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art” a prima facie case of obviousness exists.”
Regarding claims 13 and 14, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Na teaches adhering the graphene layer to a substrate such as polyethylene terephthalate (0023 and 0025). Therefore, the graphene layer will be collected as a graphene-reinforced polymer or as an aligned film because it will be aligned on the PET substrate such that the PET substrate will reinforce the graphene film. Further, the harvesting is considered to be done by an adhesive since the graphene adheres to the PET substrate.
Regarding claim 15, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Boyd further teaches using an RF plasma generator such as an Evenson cavity suitable for generating a microwave plasma to generate an RF plasma (e.g., a microwave plasma in the ultra-high frequency (UHF) portion of the RF spectrum (0023). They teach using an Evenson cavity as a plasma source for hydrogen plasma treatment with an excitation frequency of 2450 MHz, where the cavity can excite discharges in both static and flowing gases at pressures ranging from a few mTorr to several hundred Torr (0049). They teach that a benefit of this RF microwave cavity is that it can be placed directly on a quartz vacuum tube to generate plasm in situ (0049). They teach using a chamber pressure of 500 mTorr or less (0054). From this, 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 used an Evenson cavity to also generate the plasma in the continuous process because Boyd teaches that such a cavity provides benefits and can be used to generate a plasma at the desired pressure such that it will be expected to provide a suitable plasma in the low-pressure reactant gas discharge process of Boyd. It is noted that since Boyd teaches using a pressure overlapping the ranges of claims 9 and 10 (as discussed above), the process is considered to be a low-pressure reactant discharge process.
Regarding claim 16, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Boyd further depicts that the rotatable substrate is rotated entirely inside the deposition chamber (Fig. 8), where the substrate is rotated on the rolls. They teach performing deposition at a reduced pressure (0054 and Fig. 6).
Cooper also depicts the rolls as being located inside of a chamber (Fig. 2).
As discussed above, Park suggests providing the entire apparatus in a vacuum chamber (0046).
From this, 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 rotated the substrate entirely in the deposition chamber in the process of Boyd in view of Na, Zaretski, Cooper, and Park of continuously growing, harvesting, and collecting the graphene because Boyd depicts such an arrangement and they teach using a reduced pressure environment for deposition, Cooper also depicts the rolls as being within a chamber, and Park suggests providing the process in a vacuum chamber such that it will be expected to contain the rolls in the chamber and maintain the pressure needed for deposition. Specifically, by keeping the substate and the rolls in the chamber it will be able to maintain the desired pressure in the chamber by having a contained environment.
Regarding claim 17, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Boyd teaches using the roll-to-roll process for the continuous production of large area graphene (0061). Zaretski teaches that the processes are scalable to accommodate large graphene films, where there is no maximum limit in the graphene size other than the one given by the equipment used to attach the adhesive tape and the equipment used to produce the graphene (0047). They teach that the equipment could be defined to handle meter scale graphene films (0047). While they do not teach the surface area of the rotatable substrate, from the teachings of Boyd in view of Na, Zaretski, Cooper, and Park, 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 surface area to be within the claimed range because Boyd teaches forming large area graphene and Zaretski teaches that there is no maximum size limit except what is limited by the equipment, where meter scale graphene can be provided such that the process is expected to be capable of being used with large area substrate to provide large area films. 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).
Further, according to MPEP 2144.04(IV)(A): In re Rose, 220 F.2d 459, 105 USPQ 237 (CCPA 1955) (Claims directed to a lumber package "of appreciable size and weight requiring handling by a lift truck" were held unpatentable over prior art lumber packages which could be lifted by hand because limitations relating to the size of the package were not sufficient to patentably distinguish over the prior art.); In re Rinehart, 531 F.2d 1048, 189 USPQ 143 (CCPA 1976) ("mere scaling up of a prior art process capable of being scaled up, if such were the case, would not establish patentability in a claim to an old process so scaled." 531 F.2d at 1053, 189 USPQ at 148.). In Gardner v. TEC Syst., Inc., 725 F.2d 1338, 220 USPQ 777 (Fed. Cir. 1984), cert. denied, 469 U.S. 830, 225 USPQ 232 (1984), the Federal Circuit held that, where the only difference between the prior art and the claims was a recitation of relative dimensions of the claimed device and a device having the claimed relative dimensions would not perform differently than the prior art device, the claimed device was not patentably distinct from the prior art device.
Regarding claim 18, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Boyd further teaches using copper as the substrate, where other materials such as nickel, platinum, iron, cobalt, ruthenium, magnesium oxide, alloys of these material, and the like can be used (0050). Therefore the surface will comprise a metal or metal alloy.
Na also teaches using metals such as nickel, cobalt, iron, platinum, gold, aluminum, chromium, copper, magnesium, manganese, rhodium, silicon, tantalum, titanium, tungsten, uranium, vanadium, and zirconium at the catalyst metal (0020).
Zaretski also teaches using copper or nickel foils as the substrate (0005).
Cooper also teaches that the belt can be made of metals (0014).
Claims 3-5 are rejected under 35 U.S.C. 103 as being unpatentable over Boyd in view of Na, Zaretski, Cooper, and Park as applied to claim 1 above, and further in view of Chiu, US 2017/0144888 A1.
Regarding claims 3-5, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Cooper teaches treating the substrate with a plasma etch or chemical clean to clean the surface prior to depositing a catalyst support (0086 and Fig. 2).
They do not teach cleaning the surface of the rotatable substrate prior to deposition of the primary carbon layer in graphene deposition.
Chiu teaches growing graphene by chemical vapor deposition where a plasma source is used to assist the decomposition of the carbon source (abstract and 0012). They teach that the surface of the substrate may be copper, nickel, ruthenium, cobalt, and a combination thereof (0027). They teach that the surface of the substrate may have been treated with oxygen plasma or hydrogen plasma prior to being loaded in the furnace (0027). They teach that oxygen plasma may serve to remove organic substances from the surface of the substrate and the hydrogen plasma may serve to reduce the native oxide film on a metallic surface of the substrate (0027).
From the teachings of Chiu, 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 modified the process of Boyd in view of Na, Zaretski, Cooper, and Park to have used an oxygen plasma cleaning process to clean the substrate surface prior to deposition of the primary carbon layer because Chiu teaches that such a treatment helps to remove organic substances from a surface that can be copper or nickel prior to deposition of a graphene layer such that it will be expected to clean the surface for deposition. The oxygen plasma is considered to be a plasma etching process because it removes substances from the substrate surface.
While they do not teach the time period for the plasma etching process, 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 process to be within the claimed range so as to provide a plasma treatment sufficient for cleaning the surface but not overly long to reduce the efficiency of the process or to plasma damage the substrate surface. 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).
Claim 4 is alternatively rejected under 35 U.S.C. 103 as being unpatentable over Boyd in view of Na, Zaretski, Cooper, Park and Chiu as applied to claim 3 above, and further in view of Johnson, US 2016/0176755 A1.
Regarding claim 4, Boyd in view of Z Na, Zaretski, Cooper, Park, and Chiu suggest the process of claim 3, where Chiu suggests using an oxygen plasma to clean a substrate surface that may be an insulating material such as glass or a metal such as copper or nickel (0027).
They do not teach the time needed to clean the surface.
Johnson teaches methods for transferring high-quality CVD monolayers of graphene from metal substrates to flexible glass targets (abstract). They teach cleaning the glass surfaces with an oxygen plasma treatment (0005, 0040, and 0041). They teach that the oxygen plasma treatment is done at a power sufficient to generate a plasma that actively and efficiently cleans the target surface in a reasonable time period, but does not damage the surface (0041). They teach that typical cleaning durations are on the order of minutes, from about 1 min to about 30 min, from about 2 mins to about 10 mins, or about 2 mins to about 5 mins (0041).
From the teachings of Johnson, 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 oxygen plasma time to be from about 2 min to about 5 mins so as to be within the claimed range because Johnson teaches that such time durations are typically suitable for performing an oxygen plasma clean of a substrate such that it will be expected to provide a suitable plasma treatment for cleaning the substrate surface prior to deposition. 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.” Titanium Metals Corp.v. Banner, 778 F.2d 775, 227 USPQ 773 (Fed. Cir. 1985) (citing In re Petering, 301 F.2d 676, 682, 133 USPQ 275, 280 (CCPA 1962)) (emphasis in original). 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).
Claim 6 is rejected under 35 U.S.C. 103 as being unpatentable over Boyd in view of Na, Zaretski, Cooper, and Park as applied to claim 1 above, and further in view of Yeh, WO 2014/110446 A2.
The second inventor has been used for WO 2014/110446 A2 to differentiate between Boyd references.
Regarding claim 6, Boyd in view of Na, Zaretski, Cooper, and Park suggest the process of claim 1. Boyd teaches using a copper substrate (0019 and Fig. 8).
They do not teach etching the surface via cyano radicals.
Yeh teaches a method of forming graphene by placing a substrate in a processing chamber and introducing a cleaning gas including hydrogen and nitrogen into the processing chamber (abstract). They teach introducing a carbon source into the chamber and initiating a microwave plasma in the chamber so as to subject the substrate to a flow of the cleaning gas and the carbon source for a predetermined period of time to form the graphene (abstract). They teach that the cleaning gas includes cyano radicals (0007 and 0049). They teach that the flow of the cleaning gas including hydrogen and nitrogen as well as the carbon source gas creates creative species (e.g., atomic hydrogen, cyano radicals, and reactive carbon species) in the plasma (0054). They teach that the reactive species act as a cleaning gas to remove native species on the substrate and etch copper as well as depositing graphene on the substrate as the simultaneous removal of copper oxide and the deposition of graphene occurs (0054).
From the teachings of Yeh, 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 included cyano radicals in the plasma process of Boyd in view of Na, Zaretski, Cooper, and Park because Yeh teaches that having such radicals in a plasma during deposition of graphene results in cleaning a copper surface by etching the copper during deposition such that it will be expected to help clean the surface during the deposition process. Therefore, the surface of the rotatable substrate comprises copper and the surface will be etched using cyano radicals.
Response to Arguments
Applicant’s arguments, dated 12/31/2025, have been fully considered.
In light of the amendments to claim 1, the previous rejection has been modified as indicated above.
Regarding Applicant’s arguments over Zaretski, the suggestion was to peel the graphene and metal layer from the copper surface at a temperature of less than 100°C so that the thermal adhesive was not deactivated so that the graphene would be lifted from the copper surface as in step 4 of Fig. 1 of Zaretski.
As to the interpretation of the conditions being unchanged, page 7, lines 12-25 of the instant specification indicate that the conditions, i.e., temperature and pressure, during cleaning are substantially the same as during depositing the primary carbon layer and the graphene layer. Therefore, the conditions being unchanged during the process were interpreted as being the temperature and pressure.
As to Applicant’s arguments over He, since this reference is no longer used, these arguments are not addressed herein.
Regarding Applicant’s argument over the “shared atmosphere”, as discussed in the 112(a) and 112(b) rejections above, it is not clear what is required for a “shared atmosphere”. The rejection above is considered to suggest this feature because the process is done in the same vacuum chamber to provide a “shared atmosphere”.
Conclusion
Applicant's amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a).
A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to CHRISTINA D MCCLURE whose telephone number is (571)272-9761. The examiner can normally be reached Monday-Friday, 8:30-5:00 EST.
Examiner interviews are available via telephone, in-person, and video conferencing using a USPTO supplied web-based collaboration tool. To schedule an interview, applicant is encouraged to use the USPTO Automated Interview Request (AIR) at http://www.uspto.gov/interviewpractice.
If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Gordon Baldwin can be reached at 571-272-5166. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300.
Information regarding the status of published or unpublished applications may be obtained from Patent Center. Unpublished application information in Patent Center is available to registered users. To file and manage patent submissions in Patent Center, visit: https://patentcenter.uspto.gov. Visit https://www.uspto.gov/patents/apply/patent-center for more information about Patent Center and https://www.uspto.gov/patents/docx for information about filing in DOCX format. For additional questions, contact the Electronic Business Center (EBC) at 866-217-9197 (toll-free). If you would like assistance from a USPTO Customer Service Representative, call 800-786-9199 (IN USA OR CANADA) or 571-272-1000.
/CHRISTINA D MCCLURE/Examiner, Art Unit 1718
/GORDON BALDWIN/Supervisory Patent Examiner, Art Unit 1718