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 .
DETAILED ACTION
Priority
The Examiner recognizes Foreign Priority to FR2108108, with a filing date of 07/26/2021.
Information Disclosure Statement (IDS)
The information disclosure statements (IDS) submitted on 01/24/2024 and 03/30/2026 is/are in compliance with the provisions of 37 CFR 1.97. Accordingly, the information disclosure statements are being considered by the examiner. Please refer to applicant’s copy of the 1449 herewith.
Drawings
The drawings are objected to because of the minor informalities listed below:
Figures, when more than one (1) figure, are to be labeled “FIG. X” where X is an Arabic numeral. For example, “Fig. 1” should read “FIG. 1”. FIG. 1 – FIG. 2 need amending.
Corrected drawing sheets in compliance with 37 CFR 1.121(d) are required in reply to the Office action to avoid abandonment of the application. Any amended replacement drawing sheet should include all of the figures appearing on the immediate prior version of the sheet, even if only one figure is being amended. The figure or figure number of an amended drawing should not be labeled as “amended.” If a drawing figure is to be canceled, the appropriate figure must be removed from the replacement sheet, and where necessary, the remaining figures must be renumbered and appropriate changes made to the brief description of the several views of the drawings for consistency. Additional replacement sheets may be necessary to show the renumbering of the remaining figures. Each drawing sheet submitted after the filing date of an application must be labeled in the top margin as either “Replacement Sheet” or “New Sheet” pursuant to 37 CFR 1.121(d). If the changes are not accepted by the examiner, the applicant will be notified and informed of any required corrective action in the next Office action. The objection to the drawings will not be held in abeyance.
Specification
The Specification is objected to for the following informalities:
Where Claim 1 uses the phrase “amorphous carbon residue”, the Specification is replete with the terms “carbon residue” and “amorphous carbon”, which do not support the Claim 1 of “amorphous carbon residue”.
Appropriate correction is required.
Claim Interpretation
Regarding Claim 1- “and a step of carbon reduction of the silicon oxycarbide and silica present on the surface of the silicon carbide particles by the carbon residue” is understood to mean any process that reduces surface oxides, which is inherent in any high-temperature pyrolysis of materials that contain carbon, when those materials are in contact with silicon oxycarbide and/or silica.
Regarding Claim(s) 2, 4, and 5 – the claimed ranges for respective attributes are inclusive. Example: Claim 2 – slurry comprises between 1 wt.% and 20 wt.% includes 1 wt.% and 20 wt.% values.
General Note: The art does not recognize any distinction between coating and impregnating. In re Marra et al., 141 USPQ 221.
Regarding Claim 1, the term “infiltrating” can be considered impregnating.
Examiner Note: A method is defined as a series of actions (MPEP 2106 (I), i.e., “processes…defines “actions”; inventions that consist of a series of steps or acts to be performed). Thus, since methods are defined by actions, the method is given weight only to the extent that it impacts the method in a manipulative sense. See Ex parte Pfeiffer, 135 USPQ 31, noting “recited structural limitations must affect method in manipulative sense and not amount to mere claiming of a use of a particular structure”. Below is/are a list of claims/limitations that are structural limitations or mere outcomes of the method, (not a method):
Regarding an aspect of Claim 1 – “and a step of carbon reduction of the silicon oxycarbide and silica present on the surface of the silicon carbide particles by the carbon residue” is a functional step for a result of the method, not a method.
Regarding an aspect of Claim 4 – “the fibrous preform comprises between 0.001% and 0.25% by weight amorphous carbon after the step of pyrolysis of the organic binder” is a structural result of a method, not a method.
Claim Objections
Claim(s) 1 and 5 is/are objected to because of the following informalities. The form below is read/Examiner suggestion:
Regarding Claim 1 – consolidating the fibrous preform by gas-phase chemical infiltration/ consolidating the fibrous preform by gas-phase chemical infiltration forming a consolidated fibrous preform; densifying by infiltrating the preform / densifying by infiltrating the consolidated fibrous preform ;
particles by the carbon residue /particles by the amorphous carbon residue.
Regarding Claim 5 – for a duration of between 1 and 5 hours / for a duration of between 1 hour and 5 hours.
Claim Rejections - 35 USC § 103
The following is a quotation of pre-AIA 35 U.S.C. 103(a) which forms the basis for all obviousness rejections set forth in this Office action:
(a) A patent may not be obtained though the invention is not identically disclosed or described as set forth in section 102, if the differences between the subject matter sought to be patented and the prior art are such that the subject matter as a whole would have been obvious at the time the invention was made to a person having ordinary skill in the art to which said subject matter 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 pre-AIA 35 U.S.C. 103(a) 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 under pre-AIA 35 U.S.C. 103(a), the examiner presumes that the subject matter of the various claims was commonly owned at the time any inventions covered therein were made absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and invention dates of each claim that was not commonly owned at the time a later invention was made in order for the examiner to consider the applicability of pre-AIA 35 U.S.C. 103(c) and potential pre-AIA 35 U.S.C. 102(e), (f) or (g) prior art under pre-AIA 35 U.S.C. 103(a).
Claims 1-4, 6-7 is/are rejected under 35 U.S.C. 103 as being unpatentable over USPGPUB
20200199033A1 by Shim et. al. (herein “Shim”) in further view of USPGPUB 20130287941A1 by Gray
(herein “Gray”) and in further view, as supported by evidentiary reference, “ Silicon oxycarbide
formation on SiC surfaces and at the SiC/SiO2 interface” by Onneby et. al.(herein “Onneby”).
Regarding Claim 1 – Shim teaches a method for manufacturing a ceramic matrix composite part comprising,
producing a fibrous preform from silicon carbide fibres; [0024], “CMC substrate 12 includes reinforcement material…reinforcement material may include…fibers…such as SiC”.
consolidating the fibrous preform by gas-phase chemical infiltration; [0025], “…reinforcement material may include fibers coated…with an interface material…used to densify the CMC substrate prior to the application of the first slurry…the fiber interface material…may be deposited on the fibers using…chemical vapor deposition”.
injecting a slurry comprising a silicon carbide particle powder into the consolidated fibrous preform; [0026], [0029], “…first solid particles deposed on inner spaces of CMC substrate 12 using a first slurry. The first solid particles may include SiC…”, “…first solid particles maybe deposited from a first slurry using a suitable slurry infiltration technique…”
densifying by infiltrating the preform with a composition based on molten silicon to give a part made of ceramic matrix composite material; [0064], [0065], FIG. 3 , “The technique included infiltrating…with a molten infiltrant to form a composite CMC article.”, “…the melt infiltration process may densify the resultant composite article”, “…the molten metal infiltrant may include Si…”
the slurry further comprises at least one organic binder; [0028], “…the…slurry may include…additives…”, “…the additives may include a binder…”
Shim teaches the use of SiC particles in the slurry but does not disclose,
the silicon carbide particles comprising silicon oxycarbide and silica on their surface;
Evidentiary reference Onneby teaches that silicon carbide particles would inherently have silicon oxycarbide and silica on their surfaces when exposed to air (Abstract, lines 6-7). Thus such is present in the teachings of Shim.
While Shim discloses prior to melt infiltration binder may be removed through thermal burn-off ([0044], lines 29-31) Shim does not disclose,
And, in that the method comprises, before the infiltration of the preform with a composition based on molten silicon,
a step of forming an amorphous carbon residue by pyrolysing the organic binder;
and a step of carbon reduction of the silicon oxycarbide and silica present on the surface of the silicon carbide particles by the carbon residue.
In a similar endeavor of a process of producing silicon-containing CMC articles with SiC fibers ([0004]), where the process entails producing a matrix slurry composition that contains at least one resin binder and a SiC powder where a preform is impregnated with the matrix slurry [0016] and then melt infiltrated with molten silicon (Abstract), Gray discloses a CMC porous preform is produced by firing a slurry impregnated fiber reinforcement material (the preform) with subsequent molten silicon infiltration [0016]. Further, firing the preform converts at least the one resin binder to char (amorphous carbon) ([0010]). Continuing, the preform is heated (fired) in a vacuum or inert atmosphere to decompose binders ([0005], [0018]).
Gray cites that during melt infiltration, molten silicon reacts with the char to form SiC in the porous preform. As it has been established that SiC particles have silicon oxy carbide (SiOC) and silica (SiO2) on the surface of the particles, the char would then react with silicon oxy carbide (SiOC) and silica (SiO2) to form SiC, which is considered a carbon reduction process. It would have been obvious to one of ordinary skill in the art at the time of the effective filing date of the claimed invention to use the heating process before melt infiltration of Gray to create char from only resin binder in the method of Shim, as one would be motivated to do so for the purposes of ensuring there is absent unreacted carbon (char) and there is absent unfilled porosity after melt infiltration (due to too much SiC formation from excess char available), as noted by Gray [0007].
Regarding Claim 2 - Shim, Gray, and Onneby in the rejection of claim 1 above teaches all of the
limitations of claim 1. Shim teaches wherein,
the slurry comprises between 1% and 20% by weight organic binder; [0028],[0030] “…the first slurry may include…additives…”, “…the additives may include a binder…”, “…the first slurry may be formulated to include…10% percent by weight of additives (e.g. 8% by weight carbon material (binder)”.
Regarding Claim 3 - Shim, Gray, and Onneby in the rejection of claim 1 above teaches all of the
limitations of claim 1. Shim teaches wherein,
the organic binder is chosen from one of the following binders: polyvinyl alcohol (PVA), polyethylene glycol (PEG), glycerol, polymethylmethacrylate (PMMA), acrylic resin and polyvinyl butyral resin (PVB); [0028], “…the first slurry may include…additives…”, “…the additives may include a binder (e.g. …polyvinyl butyral…)”.
Regarding Claim 4 - Shim, Gray, and Onneby in the rejection of claim 1 above teaches all of the
limitations of claim 1.
While Shim teaches an organic binder content of 8% [0030] and a first slurry that carries up to 65% by
weight of first solid particles [0031], Shim does not disclose,
the fibrous preform comprises between 0.001% and 0.25% by weight amorphous carbon after
the step of pyrolysis of the organic binder.
Gray discloses slurry matrix composition produced during the investigation leading to the invention,
where SiC powder content = 78 wt%, primary resin = 15wt% and pore former = 7 wt%, where the
primary resin +pore former (char sources with the primary resin the predominant source) char yield is at
least 9.5 wt% [0018], [0019]. A PHOSITA can calculate on a gram basis where 9.5% of 22 wt% is 2.09g,
which is 2.6 wt% char (amorphous carbon as known in the art by PHOSITA) in the fibrous preform. The
amount of char is a result effective variable (reacts with SiOC and SiO2 on the surface of the SiC particles
to promote filling preform porosity during melt infiltration [0007]. Gray discloses the claimed invention
except for char yield for the binder type of Shim. It would have been obvious to one having ordinary
skill in the art at the time of the effective filing date of the claimed invention to optimize the amount of
primary resin and the char yield of Gray to the binder type/char yield of Shim, since it has been held that
discovering an optimum value of a result effective variable involves only routine skill in the art. One
would have been motivated to optimize the char yield for the binder of Shim for the purpose of
accommodating other resins (binders) such that appropriate primary binders can serve to control the
reaction so large amounts of SiC are not formed quickly during melt filtration as well as generate a
controlled amount of char and open porosity to promote molten silicon infiltration as a result of
inhibiting choking during infiltration, as noted by Gray [0020], [0021], [0022]. A particular parameter
must first be recognized as a result-effective variable, i.e., a variable which achieves a recognized result,
before the determination of the optimum or workable ranges of said variable might be characterized as
routine experimentation, In re Antonie, 559 F.2d 618, 195 USPQ 6 (CCPA 1977). Further, it is well settled
that determination of optimum values of cause effective variables such as these process parameters is
within the skill of one practicing in the art. In re Boesch, 205 USPQ 215 (CCPA 1980).
Regarding Claim 6 - Shim, Gray, and Onneby in the rejection of claim 1 above teaches all of the
limitations of claim 1.
Shim teaches wherein further comprising,
before densifying, depositing on the fibres of the fibrous preform, an interphase of pyrolytic
carbon, boron nitride or silicon-doped boron nitride; ; [0025], “…reinforcement material may
include fibers coated…with an interface material…the fiber interface material may
include…boron nitride…”
Regarding Claim 7 - Shim, Gray, and Onneby in the rejection of claim 1 above teaches all of the
limitations of claim 1.
Shim teaches wherein,
a method comprising manufacturing a blade, a nozzle, a turbine ring or a combustion chamber of a gas turbine with the method of claim 1; [0023], “…article 10 may be …a blade…a
combustion chamber liner…of a gas turbine engine”.
Claims 5 is/are rejected under 35 U.S.C. 103 as being unpatentable over Shim et. al. in further view of
Gray and in further view of U.S. Patent 6,258,737 by Steibel et. al. (herein “Steibel”) and in further view
of NPL “ Pyrolysis of polyvinyl butyral (PVB) binder in thermoelectric green tapes” by Salam et. al. (herein
“Salam”).
Regarding Claim 5 - Shim, Gray, and Onneby in the rejection of claim 1 above teaches all of the
limitations of claim 1. While Shim, Gray, and Onneby teach the use of polyvinyl butyral ([0028], TABLE
1, respectively), and Gray teaches a pyrolysis process step [0018], yet the combination does not disclose,
the pyrolysis step comprises an increase in temperature at a rate between 1 °C/min and
3°C/min;
In a similar endeavor of a method of melt infiltrating a preform with silicon, Steibel discloses (FIG. 5),
where the preform contains silicon carbide fibers is infiltrated with a slurry composition that contains at
least one high char yield resin (Col 2 lines 55-61) and silicon carbide particles (Col 3 line 26) and where
the silicon carbide fibers are coated with boron nitride before molten silicon infiltration (Col 4 lines 52-
57). Further, a pyrolysis process to burn out polyvinyl butyral and furfuryl resin ( a known in the art high
char resin) at a high char heating rate of 3°C/min up to 450°C. Heating rate can be considered a result
effective variable as the amount of char after pyrolysis relates to the ability of the molten silicon to
infiltrate the CMC. Steibel discloses the claimed invention except for pyrolysis of polyvinyl butyral only.
It would have been obvious to one having ordinary skill in the art at the time of the effective filing date
of the claimed invention to optimize the pyrolysis heating rate of Steibel for the polyvinyl butyral only
pyrolysis method of the combination, as one would be motivated to do so for the purpose of not heating
too fast to cause excess gas evolution from the decomposition of the binder that could damage the
integrity of the preform, as noted by Steibel (Col 9 lines 36-38). A particular parameter must first be
recognized as a result-effective variable, i.e., a variable which achieves a recognized result, before the
determination of the optimum or workable ranges of said variable might be characterized as routine
experimentation, In re Antonie, 559 F.2d 618, 195 USPQ 6 (CCPA 1977). Further, it is well settled that
determination of optimum values of cause effective variables such as these process parameters is within
the skill of one practicing in the art. In re Boesch, 205 USPQ 215 (CCPA 1980).
While Steibel would reasonably have a hold time duration of a peak temperature for the pyrolysis
process (it is common in the art of thermal processing to have some level of hold time at a
peak temperature), Steibel does not disclose,
to a temperature plateau between 300°C and 500°C;
the temperature plateau being maintained for a duration of between 1 and 5 hours.
In an analogous endeavor of pyrolysis of polyvinyl butyral in unfired/green ceramics to control char, Salam teaches pyrolysis of PVB at 450°C for 5hrs (Abstract line 9). Salam discloses the claimed invention except for use for CMC articles. Peak temperature and duration can be considered a result effective variable as the amount of char after pyrolysis relates to the ability of the molten silicon to infiltrate the CMC. It would have been obvious to one having ordinary skill in the art at the time of the effective filing date of the claimed invention was made to optimize the peak temperature and duration of Salam for the CMC material of the combination, as one would be motivated to do so for the purpose of reducing char, as noted by Salam (Abstract, line 9 “reduce char residue to only 1%”). A particular parameter must first be recognized as a result-effective variable, i.e., a variable which achieves a recognized result, before the determination of the optimum or workable ranges of said variable might be characterized as routine experimentation, In re Antonie, 559 F.2d 618, 195 USPQ 6 (CCPA 1977). Further, it is well settled that determination of optimum values of cause effective variables such as these process parameters is within the skill of one practicing in the art. In re Boesch, 205 USPQ 215 (CCPA 1980).
Conclusion
The prior art made of record and not relied upon is considered pertinent to the applicant’s disclosure.
Waggoner et. al. (USPGPUB 20030180579A1) – teaches (Abstract) a silicon carbide composite made by a molten silicon infiltration. Further, a binder is used as a carbon source to enhance infiltration [0021] by reacting with the molten silicon to produce SiC [0026].
Landwehr (USPGPUB 20160159698) teaches (Abstract) a method top prepare a ceramic matrix composite with ceramic powders in a slurry that infiltrates a preform. Further, the preform contains coated fiber by chemical vapor deposition [0018] and the ceramic powders contain silicon carbide with melt infiltration is cited [0012].
Gray (U.S. Patent 7,686,990) teaches (Abstract) a method of producing a ceramic matrix composite with a fiber reinforcement material with carbonaceous coating applied to the surface where the coating is a slurry containing ceramic particulate. Further, the slurry contains silicon carbide particles (Col 3 line 57), the preform is melt infiltrated with molten silicon (Col 5 lines 27, 32-33) , and carbon in the coating reacts to form SiC (Col 5 lines 38-40).
Borom et. al (U.S. Patent 5, 015, 540) teaches (Abstract) a fibrous material coated with boron nitride admixed with infiltration promoting material that contains elemental carbon that is formed into a preform and is infiltrated with molten silicon. Further, the fibrous material contains SiC (Col 2 lines 45-48) and the boron nitride coating is deposited by chemical vapor deposition (Col 4 lines 59-63), the infiltration promoting material is slurry that contains a powder (Col 5 lines 52-68) and a resin (Col 6 line 2).
Kirby (USPGPUB 20180194690A1) teaches (Abstract) a method of forming a ceramic matrix composite that is melt infiltrated where a carbon yielding resin is in the open pore channels of the preform where upon heating, reacts with silicon to form SiC. Further, molten silicon is used for melt infiltration [0012], fiber coatings are applied by chemical vapor infiltration and the preform is heated to decompose the organic binders to carbon char [0028].
Bouillon et. al. (USPGPUB 20150008613A1) teaches (Abstract) a method of forming a ceramic matrix composite by making a consolidated fiber preform, the fibers of the preform being carbon or ceramic fibers that are coated in an interphase formed by at least one layer of pyrolytic carbon (PyC) or of boron-doped carbon (BC). Obtaining a partially densified consolidated fiber preform, where partial densification comprises forming a first matrix phase on the interphase, the first matrix phase comprising a plurality of layers of self-healing material alternating with one or more layers of PyC or of BC. Continuing densification by dispersing carbon and/or ceramic powder within the partially densified consolidated preform and by infiltrating molten silicon or a liquid composition formed for the most part of silicon. Further, the interphase material coating in the fibers is performed by chemical vapor infiltration [0026].
Any inquiry concerning this communication or earlier communications from the examiner should be directed to CHRISTOPHER PAUL DAIGLER whose telephone number is (571)272-1066. The examiner can normally be reached Monday-Friday 7:30-4:30 CT.
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/CHRISTOPHER PAUL DAIGLER/ Examiner, Art Unit 1741
/ALISON L HINDENLANG/Supervisory Patent Examiner, Art Unit 1741
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