DETAILED ACTION
An Office Action was mailed 06/03/2025.
Applicant filed a response on 12/03/2025, and amended claims 1, 7, 19 and 23.
Claims 1-32 are pending. Claims 1-8 and 19-24 are rejected. Claims 9-18 and 25-32 are withdrawn from consideration.
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
The specification at page 7, line 5-page 8, line 15 defines the term “graphene:”
“For purposes of this disclosure, graphene refers to the broad category of single-layer allotropes of carbon, which are arranged in a two-dimensional hexagonal, or honeycomb lattice …
In any sense, the individual layers or stacks of layers of graphite of any type-graphite, graphite oxide, or graphite with other functional groups-may be known simply as graphene in the art…
As such, graphene as used herein refers to the broad category of single-layer allotropes of carbon as described above and herein.”
As defined in the specification, the term “graphene” as claimed will be examined as including graphene, graphene oxide, and graphene with other functional groups.
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 and 19 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Tian et al, CN 112408827A (Tian), taken in view of evidence by Encyclopedia Britannica, “Graphene” (Britannica) with respect to claim 19.
The machine translation of Tian provided with the PTO-892 mailed 06/03/2025 is referenced in the below rejections.
Regarding claims 1 and 19, Tian teaches a recycled concrete comprising: a) recycled aggregate, cement and water (i.e., concrete mixture), a nano strengthening liquid comprising b) nano SiO2 which is emulsified and dispersed (i.e., colloidal silica admixture) and c) GNP in water (i.e., nanographene or an aqueous graphene admixture), and d) steel fiber-PVA hybrid fiber (Tian; page 2, lines 20-41).
Although Tian does not explicitly teach “a graphene admixture in an aqueous solution that is prepared independently from the colloidal silica admixture”
as presently claimed, it is noted that the present claims are drawn to a product and not drawn to a method of making. Thus, “[E]ven though product-by-process claims are limited by and defined by the process, determination of patentability is based on the product itself. The patentability of a product does not depend on its method of production. If the product in the product-by-process claim is the same as or obvious from a product of the prior art, the claim is unpatentable even though the prior product was made by a different process”, In re Thorpe, 777 F.2d 695, 698, 227 USPQ 964, 966 (Fed. Cir. 1985). Further, “although produced by a different process, the burden shifts to applicant to come forward with evidence establishing an unobvious difference between the claimed product and the prior art product”, In re Marosi, 710 F.2d 798, 802, 218 USPQ 289, 292 (Fed. Cir.1983). See MPEP 2113.
Therefore, absent evidence of criticality regarding the presently claimed “graphene admixture in an aqueous solution that is prepared independently from the colloidal silica admixture,” and given that Tian meets the requirements of the claimed product, including a concrete product comprising an aqueous graphene admixture, Tian clearly meets the requirements of the present claim.
The nano-strengthened liquid, water and cement are admixed to form a slurry, which is then mixed with the other components to prepare a recycled concrete (i.e., a concrete product set by pouring a concrete slurry) (Tian; page 4, line 59-page 5, line 6). Although Tian does not explicitly teach pouring and setting of the concrete product, Tian performs compressive and flexural strength tests on the produced concrete (Tain; page 9, lines 17-19). It is clear that the concrete would be poured and set prior to performing such tests.
Product-by-process claims are not limited to the manipulations of the recited steps, only the structure implied by the steps. Once a product appearing to be substantially identical is found and a prior art rejection is made, the burden shifts to Applicant to show an obvious difference. See MPEP 2133.
The nano strengthening liquid also contains nano CaCO3. The nano SiO2 and nano CaCO3 can effectively promote cement hydration to form CHS gel (i.e., calcium silicate hydrate gel), filling the micropores of the recycled concrete and increasing the density (i.e., wherein the silica and lime at least partially fill the capillary structures of the concrete, and react to produce a gel structure of calcium silicate hydrate that at least partially fills the capillary structures) (Tian; page 2, lines 53-54).
The oxygen-containing groups on the nano-GNP (nanographene) have a template and filling effect on the formation of cement products, which can optimize the shape and improve the compactness of the cement product, and improve the mechanical properties of the recycled concrete (Tian; page 2, lines 55-59).
Tian repeatedly teaches that the nano-scaled materials are fully dispersed throughout the concrete, filling the harmful pores, and improving the mechanical properties, including compressive and flexural strength (Tian; page 2, lines 47-59; page 3, lines 2-4, 12-14 and 24-28; page 4, lines 33-36; page 3, line 59-page 4, line 69, lines 11-49).
Because Tian teaches concrete products comprising components, including graphene in the nano strengthening liquid, that are substantially identical to the components used in the concrete product of the present invention, as set forth above, the resulting concrete products of Tian would inherently possess the properties as claimed, i.e. reduced internal tensile forces acting on the concrete product, and wherein the graphene in Tian would inherently distribute the load of the composite material acting on the concrete product.
Regarding claim 19, Brittanica teaches that graphene is a two-dimensional form of crystalline carbon, existing either as a single layer or several coupled layers (i.e., overlapping). The word “graphene” when used without specificizing the form generally refers to single layer graphene (Britannica; page 1, para 1). As is evidenced by Britannica, it is clear that the graphene in Tian would necessarily exist as a monolayer or as coupled/overlapped layers in the concrete products of Tian.
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). See MPEP 2112.01 (I).
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.
Claims 7-8 and 23-24 are rejected under 35 U.S.C. 103 as being unpatentable over Tian.
Regarding claims 7 and 23, Tian is relied upon as teaching the limitations of claims 1 and 19 as discussed above. Tian teaches that the concrete contains 70-130 parts of cement, and 35-75 parts of water (i.e., a water to cement ratio of 0.26 to 1.07) (Tian; page 2, lines 24 and 28). These amounts overlap in scope with the claimed water to cement ratio of 0.40 to 0.45.
As set forth in MPEP 2144.05, in the case where the claimed range “overlap or lie inside ranges disclosed by the prior art”, a prima facie case of obviousness exists, In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990).
Regarding claims 8 and 24, Tian is relied upon as teaching the limitations of claims 1 and 19 as discussed above. Tian teaches that 0.84 to 1.8 parts of the steel fiber-PVA hybrid fiber is added to the recycled concrete product (Tian; page 2, line 30).
Tian does not explicitly teach wherein the steel and PVA fibers are added in an amount of about 0.2% to about 0.5% by volume of the poured concrete slurry. However, Tian teaches that the steel and PVA fibers, together with the waste textile fiber, emery, soy protein and trehalose, synergize to fully fill the harmful pores of the recycled concrete and improve the mechanical properties (Tian; page 3, lines 1-4).
It has long been an axiom of United States patent law that it is not inventive to discover the optimum or workable ranges of result-effective variables by routine experimentation. In re Peterson, 315 F.3d 1325, 1330 (Fed. Cir. 2003) ("The normal desire of scientists or artisans to improve upon what is already generally known provides the motivation to determine where in a disclosed set of percentage ranges is the optimum combination of percentages."); In re Boesch, 617 F.2d 272, 276 (CCPA 1980) ("[D]iscovery of an optimum value of a result effective variable in a known process is ordinarily within the skill of the art."); In re Aller, 220 F.2d 454, 456 (CCPA 1955) ("[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."). "Only if the 'results of optimizing a variable' are 'unexpectedly good' can a patent be obtained for the claimed critical range." In re Geisler, 116 F.3d 1465, 1470 (Fed. Cir. 1997) (quoting In re Antonie, 559 F.2d 618, 620 (CCPA 1977)).
It would have been obvious to one of ordinary skill in the art to vary the %volume of steel and PVA fibers, including over the presently claimed, in order to fully fill the pores and thereby improve the mechanical properties of the recycled concrete product of Tian.
Claims 1, 7-8, 19-20 and 23-24 are rejected under 35 U.S.C. 103 as being unpatentable over Adams, US 2020/0087202 A1 (Adams) in view of Zhao et al, “Synergistic effects of silica nanoparticles/polycarboxylate superplasticizer modified graphene oxide on mechanical behavior and hydration process of cement compositions” (Zhao).
Regarding claim 1, Adams teaches a concrete slab (i.e., product) set by pouring a concrete slurry onto a substrate, the concrete slurry comprising a) a concrete mixture; b) a colloidal silica mixture; and c) at least one fiber selected from steel fibers and synthetic fibers, both of which fall within the claimed fiber component d) (Adams; [0013] and claim 1). As the poured concrete slurry cures, the poured concrete slurry hardens into a composite material taking the form of a jointless concrete slab, the jointless concrete slab defines capillary structures that at least in part fill with silica particles and lime. The silica particles and lime react therein to produce a gel structure of calcium silicate hydrate that at least partially fills the capillary structures, and that reduces the internal tensile forces acting on the concrete slab (Adams; [0013] and claim 1). The silica particles have a size of 10-100nm, i.e., they are nanoparticles (Adams; [0014]).
Adams does not explicitly teach the addition of a graphene admixture in an aqueous solution that is prepared independently from the colloidal silica admixture to the concrete product, wherein the graphene embeds along at least partially fills the capillary structures and at least partially in part distributes the load of the composite material acting on the concrete structure.
With respect to the difference, Zhao teaches that the high specific surface area, extraordinary intrinsic strength, and good dispersion property of GO (i.e., graphene oxide) make it an attractive candidate for reinforcing cement composites. GO can accelerate cement hydration, regulate the microstructure of hydration crystals, and significantly improve the mechanical behavior of cement composites. However, it is difficult to disperse GO nanosheets in alkaline cement matrix due to electrostatic interactions (Zhao; page 16688; col. 2, lines 6-14).
SiO2 NPs (i.e., silica nanoparticles) with high specific area have been widely utilized to reinforce cement composites and have produced remarkable improvement in mechanical strength on account of nucleus and filling effects (emphasis added). Moreover, SiO2 NPs with pozzolanic activity can consume calcium hydroxide (CH) to form stable calcium silicate hydrate (C-S-H) gels. These advantages provide the motivation to hybridize SiO2 NPs with GO nanosheets for further enhancement in mechanical properties of cement composites (Zhao; page 16689, col. 1, para 1).
To enhance the mechanical behavior of cement composites, SiO2 NPs were introduced to an aqueous solution PC@GO (i.e., graphene oxide modified by polycarboxylate superplasticizer, or a graphene admixture in an aqueous solution that is prepared independently from the silica as claimed) to form SiO2 NPs/PC@GO hybrid (Zhao; Abstract and page 16696, col. 1, para 1). The pozzolanic activity of SiO2 coupled with the nano-filling effect (i.e., capillary filling effect) is in favor of the mechanical enhancement of cement composites (Zhao; page 16696, col. 1, para 1). For hybrid-cement samples it can be clearly observed of the synergistic effects of SiO2 NPs and PC@GO on cement hydration and microstructure development (Zhao; page 16696, col. 1, para 2).
The SiO2 NPs and PC@GO hybrid can accelerate cement hydration to yield compact microstructure, react to form high density C-S-H gels, the most desirable products of cement hydration and contributors to mechanical strength. The C-S-H gels develop around GO nanosheets and lead to the formation of a network structure (Zhao, page 16700, col. 2, line 12-page 16701, lines 4). A crosslinking structure is formed (SiO2-GO-CSH) using GO as the bridge, alleviating stress concentration and facilitating the load-transfer uniformity throughout the cement matrix (i.e., whereby the embedded graphene at least in part distributes the load of the composite material acting on the concrete product) (Zhao; page 16702, col. 1, first full para). In conclusion, synergistic effects of SiO2 NPs/PC@GO hybrid are obtained on the compressive strength of cement composites (Zhao; page 16702, 4. Conclusions).
In light of the motivation provided by Zhao, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to add the separately prepared, modified graphene aqueous solution to the concrete slurry of Adams in order to obtain the synergistic effects of cement hydration, microstructure development, mechanical strength, and SiO2-GO-CSH crosslinking which alleviates stress concentration and facilitates load-transfer uniformity throughout the cement matrix.
Upon performing such an addition, those skilled in the art would expect to obtain a concrete product having the claimed features and properties (i.e., wherein the capillary structures at least partially fill with graphene and wherein the embedded graphene at least partially distributes the load of the composite material acting on the concrete product) because: 1) the concrete products of Adams have capillary structures that are at least partially filled with gel calcium-silicate-hydrate, 2) the concrete slurry of Adams comprises SiO2 nanoparticles, and 3) the graphene oxide of Zhao work synergistically with SiO2 nanoparticles to provide a nano-filling effect, microstructure development, crosslinking with calcium-silicate-hydrate gel, and improved mechanical strength and load distribution.
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). See MPEP 2112.01 (I).
Regarding claim 7, Adams in view of Zhao are relied upon as teaching the limitations of claim 1 as discussed above. Adams teaches that the concrete mixture comprises aggregate, cement, and water, wherein the concrete mixture is defined by a water to cement ratio of between about 0.400 to about 0.450 as claimed (Adams; [0014] and claim 7).
Regarding claim 8, Adams in view of Zhao are relied upon as teaching the limitations of claim 1 as discussed above. Adams teaches that the at least one fiber represents between about 0.25% by volume to about 0.50% by volume of the poured concrete slurry (Adams; [0014] and claim 8). This falls completely within the claimed range 0.20-0.50% by volume.
Regarding claim 19, Adams teaches a jointless concrete slab (i.e. product) set from a concrete slurry poured onto a substrate, the poured concrete slurry comprising a concrete mixture, a colloidal silica admixture, and at least one fiber selected from the group of fibers consisting of steel fibers and synthetic fibers, the jointless concrete slab comprising capillary structures that are at least in part filled with a reaction product of silica particles and lime, the reaction product being a gel structure of calcium silicate hydrate, whereby the calcium silicate hydrate reduces internal tensile forces acting on the jointless concrete slab (Adams; [0019] and claim 19).
Adams does not explicitly teach the addition of a graphene admixture in an aqueous solution that is prepared independently from the colloidal silica admixture to the concrete slurry, wherein the graphene is embedded in the capillary structures, and wherein the embedded graphene is graphene monolayers or overlapping graphene and at least partially in part distributes the load of the composite material acting on the concrete structure.
With respect to the difference, Zhao teaches that the high specific surface area, extraordinary intrinsic strength, and good dispersion property of GO (i.e., graphene oxide) make it an attractive candidate for reinforcing cement composites. GO can accelerate cement hydration, regulate the microstructure of hydration crystals, and significantly improve the mechanical behavior of cement composites. However, it is difficult to disperse GO nanosheets in alkaline cement matrix due to electrostatic interactions (Zhao; page 16688; col. 2, lines 6-14).
SiO2 NPs (i.e., silica nanoparticles) with high specific area have been widely utilized to reinforce cement composites and have produced remarkable improvement in mechanical strength on account of nucleus and filling effects. Moreover, SiO2 NPs with pozzolanic activity can consume calcium hydroxide (CH) to form stable calcium silicate hydrate (C-S-H) gels. These advantages provide the motivation to hybridize SiO2 NPs with GO nanosheets for further enhancement in mechanical properties of cement composites (Zhao; page 16689, col. 1, para 1).
To enhance the mechanical behavior of cement composites, SiO2 NPs were introduced to an aqueous solution of PC@GO (i.e., graphene oxide modified by polycarboxylate superplasticizer or a graphene admixture in an aqueous solution that is prepared independently from the colloidal silica admixture as claimed) to form SiO2 NPs/PC@GO hybrid (Zhao; Abstract and page 16696, col. 1, para 1). The GO nanosheets used are flake-like with overlapping layers (Zhao; page 16692, 3.1, para 2).
The pozzolanic activity of SiO2 coupled with the nano-filling effect (i.e., capillary filling effect) is in favor of the mechanical enhancement of cement composites (Zhao; page 16696, col. 1, para 1). For hybrid-cement samples it can be clearly observed of the synergistic effects of SiO2 NPs and PC@GO on cement hydration and microstructure development (Zhao; page 16696, col. 1, para 2).
The SiO2 NPs and PC@GO hybrid can accelerate cement hydration to yield compact microstructure, react to form high density C-S-H gels, the most desirable products of cement hydration and contributors to mechanical strength. The C-S-H gels develop around GO nanosheets and lead to the formation of a network structure (Zhao, page 16700, col. 2, line 12-page 16701, lines 4). A crosslinking structure is formed (SiO2-GO-CSH) using GO as the bridge, alleviating stress concentration and facilitating the load-transfer uniformity throughout the cement matrix (i.e., whereby the embedded graphene at least in part distributes the load of the composite material acting on the concrete product) (Zhao; page 16702, col. 1, first full para). In conclusion, synergistic effects of SiO2 NPs/PC@GO hybrid are obtained on the compressive strength of cement composites (Zhao; page 16702, 4. Conclusions).
In light of the motivation provided by Zhao, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to add the independently prepared, aqueous solution of modified graphene oxide nanosheets to the concrete slurry of Adams in order to obtain the synergistic effects of cement hydration, microstructure development, mechanical strength, and SiO2-GO-CSH crosslinking which alleviates stress concentration and facilitates load-transfer uniformity throughout the cement matrix.
Upon performing such an addition, those skilled in the art would expect to obtain a concrete product having the claimed features and properties (i.e., wherein the capillary structures at least partially fill with graphene and wherein the embedded graphene is in monolayers or overlapping and at least partially distributes the load of the composite material acting on the concrete product) because: 1) the concrete products of Adams have capillary structures that are at least partially filled with gel calcium-silicate-hydrate, 2) the concrete slurry of Adams comprises SiO2 nanoparticles, and 3) the graphene oxide layered nanosheets of Zhao work synergistically with SiO2 nanoparticles to provide a nano-filling effect, microstructure development, crosslinking with calcium-silicate-hydrate gel, and improved mechanical strength and load distribution.
Regarding claim 23, Adams in view of Zhao are relied upon as teaching the limitations of claim 19 as discussed above. Adams teaches that the concrete mixture comprises aggregate, cement, and water, wherein the concrete mixture is defined by a water to cement ratio of between about 0.400 to about 0.450 as claimed (Adams; [0014] and claim 23).
Regarding claim 24, Adams in view of Zhao are relied upon as teaching the limitations of claim 19 as discussed above. Adams teaches that the at least one fiber represents between about 0.20% by volume to about 0.50% by volume of the poured concrete slurry as claimed (Adams; [0014] and claims 24-25).
Claims 2 and 20 are rejected under 35 U.S.C. 103 as being unpatentable over Adams in view of Zhao as applied to claims 1 and 19 above, and further in view of Reade International Corp. “Graphene Oxide (GO) Dispersion, Flake & Powder” retrieved from the Wayback Machine web archive (2016) (Reade).
Regarding claims 2 and 20, Adams in view of Zhao are relied upon as teaching the limitations of claim 1 and 19 as discussed above. Adams teaches that the colloidal silica has silica particles ranging in size from about 5nm to about 100nm (Adams; [0014]).
Adams in view of Zhao does not explicitly teach wherein the graphene oxide is 1.10 ±0.2nm thick with a lattice constant of about 0.27 nm x 0.41 nm. However, a skilled artisan would consider a variety of sources to obtain the graphene oxide disclosed by Zhao. One such source is Reade International, which commercially sold graphene oxide with 1.1 ± 0.2 nm thick layers in a rectangular pattern with lattice constant of 0.27 nm X 0.41 nm, prior to the effective filing date of the claimed invention (Reade; Description, para 3, teaching graphene oxide flakes with exact same parameters as claimed). The selection of a known material based on its suitability for its intended use is prima facie obvious. See MPEP § 2144.07.
Thus, it would have been obvious to a person of ordinary skill in the art before the effective filing date of the claimed invention to select graphene oxide from a commercially available source such as Reade, for incorporation in the concrete product of Adams in view of Zhao, and thereby arrive at the claimed invention.
Claims 3-4, 6 and 21 are rejected under 35 U.S.C. 103 as being unpatentable over Adams in view of Zhao as applied to claims 1 and 19 above, and further in view of Chen et al, CN 106699006A (Chen).
Regarding claims 3 and 21, Adams in view of Zhao are relied upon as teaching the limitations of claim 1 and 19 as discussed above. Adams further teaches applying a curing technique to the poured and set concrete slurry, the curing technique comprising spraying a secondary colloidal silica onto the poured and set concrete slurry (Adams; [0015], claim 3 and claim 21).
Adams in view of Zhao does not explicitly teach wherein the curing technique comprises spray-applying graphene.
With respect to the difference, Chen teaches two-component a concrete curing agent comprising a component A comprising and a component B, wherein component A contains a silica sol (i.e., colloidal silica) and component B comprises graphene (Chen; Abstract and page 2, lines 31-38). The curing agent is reasonable in design, has high hardness, good permeability, abrasion resistance and water repellency, and can improve the strength and hydrophobicity of the concrete structure (Chen, page 2, lines 24-27). The silica in the sol have a particle size of 10-20nm (Chen, page 2, lines 49-51). The silica sol has a strong penetration, and reacts to form calcium silicate gel, making the concrete surface denser with higher hardness and increased wear resistance (Chen; page 3, lines 22-25). The component B contains graphene and a silicone modified waterborne epoxy resin dispersed in aqueous solution, forming a dense physical insulation layer, improving the resin protection effect and corrosion resistance (Chen; page 3, lines 29-32).
In light of the motivation provided by Chen, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to modify the colloid silica curing agent in the concrete products of Adams in view of Zhao with the two-component curing agent of Chen, which includes not only the silica of Adams but also components such as the claimed graphene, in order to obtain a cement product with a dense physical insulation layer, and improved protection, corrosion resistance, hardness, wear resistance, permeability, abrasion resistance, water repellency, strength and hydrophobicity.
Regarding claim 4, Adams in view of Zhao and further in view of Chen are relied upon as teaching the limitations of claim 3 as discussed above. Adams teaches that the secondary colloidal solution (i.e., the curing solution) comprises spray-applying onto the poured concrete slurry subsequent to removal of a trowel machine (Adams; [0018] and claim 4).
Regarding claim 6, Adams in view of Zhao and further in view of Chen are relied upon as teaching the limitations of claim 3 as discussed above. Adams teaches that the secondary colloidal solution (i.e., the curing solution) comprises spray-applying onto the poured concrete slurry subsequent to cement in the poured slurry being set (Adams; [0015] and claim 6).
Claims 5 and 22 are rejected under 35 U.S.C. 103 as being unpatentable over Adams in view of Zhao and further Chen as applied to claims 3 and 21 above, and further in view of Reade.
Regarding claims 5 and 22, Adams in view of Zhao and further in view of Chen are relied upon as teaching the limitations of claims 3 and 21 respectively as set forth above. Adams teaches that the secondary silica particles have a size ranging from 10.0 to 50.0, which overlaps with the claimed range of 3.0 to 25.0nm (Adams; [0015], claims 5 and 30).
Further, Chen teaches that the silica particles are 10-20nm. Such nano-sized particles ensure even dispersion, and after curing does not affect the appearance (Chen; page 2, lines 49-51). This range falls completely within the claimed range of 3.0 to 25.0nm.
In light of the motivation provided by Chen, It would have been obvious to one of ordinary skill in the art to adjust the silica particle size in the curing solutions of Adams as modified by Chen, in order to obtain good dispersion and no noticeable appearance after curing, and thereby arrive at the claimed invention.
Adams in view of Zhao and Chen does not explicitly teach wherein the graphene is 1.10 ±0.2nm thick with a lattice constant of about 0.27 nm x 0.41 nm. However, a skilled artisan would consider a variety of sources to obtain the graphene disclosed by Chen. Further, Applicant’s specification at page 7, lines 19-21, teaches “the individual layers or stacks of layers of graphite of any type-graphite, graphite oxide, or graphite with other functional groups-may be known simply as graphene in the art.” Therefore, those skilled in the art would understand that the “graphene” of Chen includes any type of graphene, graphene oxide, or graphene with other functional groups.
One such source is Reade International, which commercially sold graphene oxide with 1.1 ± 0.2 nm thick layers in a rectangular pattern with lattice constant of 0.27 nm X 0.41 nm, prior to the effective filing date of the claimed invention (Reade; Description, para 3, teaching graphene oxide flakes with exact same parameters as claimed). The selection of a known material based on its suitability for its intended use is prima facie obvious. See MPEP § 2144.07.
Thus, it would have been obvious to a person of ordinary skill in the art before the effective filing date of the claimed invention to select graphene oxide from a commercially available source such as Reade, for incorporation in the curing solution of Adams in view of Zhao and Chen, and thereby arrive at the claimed invention.
Double Patenting
The nonstatutory double patenting rejection is based on a judicially created doctrine grounded in public policy (a policy reflected in the statute) so as to prevent the unjustified or improper timewise extension of the “right to exclude” granted by a patent and to prevent possible harassment by multiple assignees. A nonstatutory double patenting rejection is appropriate where the conflicting claims are not identical, but at least one examined application claim is not patentably distinct from the reference claim(s) because the examined application claim is either anticipated by, or would have been obvious over, the reference claim(s). See, e.g., In re Berg, 140 F.3d 1428, 46 USPQ2d 1226 (Fed. Cir. 1998); In re Goodman, 11 F.3d 1046, 29 USPQ2d 2010 (Fed. Cir. 1993); In re Longi, 759 F.2d 887, 225 USPQ 645 (Fed. Cir. 1985); In re Van Ornum, 686 F.2d 937, 214 USPQ 761 (CCPA 1982); In re Vogel, 422 F.2d 438, 164 USPQ 619 (CCPA 1970); In re Thorington, 418 F.2d 528, 163 USPQ 644 (CCPA 1969).
A timely filed terminal disclaimer in compliance with 37 CFR 1.321(c) or 1.321(d) may be used to overcome an actual or provisional rejection based on nonstatutory double patenting provided the reference application or patent either is shown to be commonly owned with the examined application, or claims an invention made as a result of activities undertaken within the scope of a joint research agreement. See MPEP § 717.02 for applications subject to examination under the first inventor to file provisions of the AIA as explained in MPEP § 2159. See MPEP § 2146 et seq. for applications not subject to examination under the first inventor to file provisions of the AIA . A terminal disclaimer must be signed in compliance with 37 CFR 1.321(b).
The filing of a terminal disclaimer by itself is not a complete reply to a nonstatutory double patenting (NSDP) rejection. A complete reply requires that the terminal disclaimer be accompanied by a reply requesting reconsideration of the prior Office action. Even where the NSDP rejection is provisional the reply must be complete. See MPEP § 804, subsection I.B.1. For a reply to a non-final Office action, see 37 CFR 1.111(a). For a reply to final Office action, see 37 CFR 1.113(c). A request for reconsideration while not provided for in 37 CFR 1.113(c) may be filed after final for consideration. See MPEP §§ 706.07(e) and 714.13.
The USPTO Internet website contains terminal disclaimer forms which may be used. Please visit www.uspto.gov/patent/patents-forms. The actual filing date of the application in which the form is filed determines what form (e.g., PTO/SB/25, PTO/SB/26, PTO/AIA /25, or PTO/AIA /26) should be used. A web-based eTerminal Disclaimer may be filled out completely online using web-screens. An eTerminal Disclaimer that meets all requirements is auto-processed and approved immediately upon submission. For more information about eTerminal Disclaimers, refer to www.uspto.gov/patents/apply/applying-online/eterminal-disclaimer.
Claims 1, 7-12, 17-20 and 23-24 are provisionally rejected on the ground of nonstatutory double patenting as being unpatentable over claims 1, 6-11, 16-19 and 22-23 of copending Application No. 17/711,493 in view of Zhao et al, “Synergistic effects of silica nanoparticles/polycarboxylate superplasticizer modified graphene oxide on mechanical behavior and hydration process of cement compositions” (Zhao).
This is a provisional nonstatutory double patenting rejection.
Regarding claims 1 and 19, copending claims 1 and 18 claim a concrete product set by pouring a concrete slurry, the poured concrete slurry comprising: a) a concrete mixture; b) a graphene admixture; and c) at least one fiber selected from the group of fibers consisting of steel fibers, helix fibers, basalt fibers, polyvinyl alcohol (PVA) fibers, carbon fibers, and synthetic fibers; wherein, as the poured concrete slurry cures, the poured slurry hardens into a composite material, the composite material defining capillary structures that at least in part fill with graphene, the embedded graphene being monolayers or overlapping layers (copending claim 18); and wherein the graphene embed along and partially fill the capillary structures; whereby the embedded graphene at least in part distribute the load of the composite material acting on the concrete product.
Copending claims 1 and 18 do not claim wherein the concrete slurry comprises a colloidal silica admixture; wherein the capillary structures least in part fill with silica and lime; wherein the silica and lime react to produce a gel structure of calcium silicate hydrate that at least partially fill the capillary structures; and whereby the calcium silicate hydrate reduces internal tensile forces acting on the concrete product.
With respect to the difference, Zhao teaches that SiO2 NPs (i.e., silica nanoparticles) with high specific area have been widely utilized to reinforce cement composites and have produced remarkable improvement in mechanical strength on account of nucleus and filling effects (emphasis added). Moreover, SiO2 NPs with pozzolanic activity can consume calcium hydroxide (CH) to form stable calcium silicate hydrate (C-S-H) gels (i.e., wherein the silica and lime react to produce a gel structure of calcium silicate hydrate that at least partially fill the capillary structures). These advantages provide the motivation to hybridize SiO2 NPs with GO nanosheets for further enhancement in mechanical properties of cement composites (Zhao; page 16689, col. 1, para 1).
The SiO2 NPs were dispersed in deionized water (i.e., colloidal) (Zhao; page 16690, 2.3, para 1). For hybrid-cement samples it can be clearly observed of the synergistic effects of SiO2 NPs and PC@GO on cement hydration and microstructure development (Zhao; page 16696, col. 1, para 2).
The SiO2 NPs and PC@GO hybrid can accelerate cement hydration to yield compact microstructure, react to form high density C-S-H gels, the most desirable products of cement hydration and contributors to mechanical strength. The C-S-H gels develop around GO nanosheets and lead to the formation of a network structure (Zhao, page 16700, col. 2, line 12-page 16701, lines 4). A crosslinking structure is formed (SiO2-GO-CSH) using GO as the bridge, alleviating stress concentration throughout the cement matrix (Zhao; page 16702, col. 1, first full para). In conclusion, synergistic effects of SiO2 NPs/PC@GO hybrid are obtained on the compressive strength of cement composites (Zhao; page 16702, 4. Conclusions).
In light of the motivation provided by Zhao, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to add the SiO2 NPs to the concrete slurry of Adams in order to obtain the synergistic effects of cement hydration, microstructure development, mechanical strength, and SiO2-GO-CSH crosslinking which alleviates stress concentration throughout the cement matrix.
Upon performing such an addition, those skilled in the art would expect to obtain a concrete product having the claimed features and properties (i.e., whereby the calcium silicate hydrate reduces internal tensile forces acting on the concrete product) because: 1) the concrete products of copending claim 1 have capillary structures that at least partially fill with graphene, 2) the concrete slurry of copending claim 1 comprises graphene and 3) the SiO2 NPs of Zhao work synergistically with graphene to provide a nano-filling effect, microstructure development, crosslinking with calcium-silicate-hydrate gel, and improved mechanical strength and load distribution.
Regarding claim 7, copending claim 6 claims wherein the concrete mixture comprises aggregate, cement, and water, and wherein the concrete mixture is defined by a water to cement ratio of between about 0.400 to about 0.450.
Regarding claim 8, copending claim 7 claims wherein the at least one fiber represents between about 0.20% by volume to about 0.50% by volume of the poured concrete slurry.
Regarding claim 9, copending claim 8 recites the claimed process of claim 9, but does not claim wherein the concrete slurry comprises a colloidal silica admixture; wherein the capillary structures least in part fill with silica and lime; wherein the silica and lime react to produce a gel structure of calcium silicate hydrate that at least partially fill the capillary structures; and whereby the calcium silicate hydrate reduces internal tensile forces acting on the concrete product.
Zhao is relied upon above as teaching the synergistic effects of combining SiO2 NPs and graphene in concrete products. Therefore, and for the reasons discussed above, it would have been obvious to one of ordinary skill in the art to add SiO2 NPs to the concrete slurry of copending claim 8 in order to obtain the synergistic effects and improved mechanical properties taught by Zhao, and thereby arrive at the claimed invention.
Regarding claim 10, copending claim 9 claims wherein the preparing step comprises preparing the concrete slurry with graphene having a size of about 1.10± 0.20 nm thick with lattice constant of about 0.27 nm x 0.41 nm.
Copending claim 9 does not claim wherein the colloidal silica has a size ranging from between about 3.0 nm to about 100.0 nm.
With respect to the difference, Zhao teaches using SiO2 with a mean particle size of 15nm, which falls completely within the claimed range of 3.0-100.0nm (Zhao; page 16689, 2.1, para 1).
Regarding claims 11 and 12, copending claims 10 and 11 claim wherein the preparing step additionally comprises adding the graphene admixture to the concrete slurry in ranges of between about 0.01% to about 0.10% by weight of cement.
Copending claims 10 and 11 do not claim adding the colloidal silica admixture to the concrete slurry in ranges of between about 0.50% to about 1.50% by weight of cement in the concrete mixture.
However, Zhao teaches adding SiO2 in an amount of 0.1% by weight of the cement, which falls completely within the claimed range (Zhao; page 16691; Table 3).
Regarding claim 17, copending claim 16 claims wherein the preparing step comprises preparing the concrete slurry for pouring with dosages of steel fibers as the at least one fiber selected from the group of fibers of between about 33.0 pounds per cubic yard (lbs./cuyd) to about 66.0 lbs./cuyd.
Regarding claim 18, copending claim 17 claims wherein the preparing step comprises preparing the concrete slurry for pouring with dosages of helix fibers, basalt fibers, PVA fibers, or carbon fibers, as the at least one fiber selected from the group of fibers, of between about 3.0 lbs./cuyd to about 7.5 lbs./cuyd, or about 3.0 lbs./cuyd to about 35.0 lbs./cuyd if helix fibers.
Regarding claim 20, copending claim 19 claims wherein the graphene are about 1.10 + 0.20 nm thick with lattice constant of about 0.27 nm x 0.41 nm.
Copending claim 19 does not claim wherein the silica has a size ranging from between about 3.0 nm to about 100.0 nm. However, Zhao teaches adding SiO2 in an amount of 0.1% by weight of the cement, which falls completely within the claimed range (Zhao; page 16691; Table 3).
Regarding claim 23, copending claim 22 claims wherein the concrete mixture comprises aggregate, cement, and water, and wherein the concrete mixture is defined by a water to cement ratio of between about 0.400 to about 0.450.
Regarding claim 24, copending claim 23 claims wherein the at least one fiber represents between about 0.20% by volume to about 0.50% by volume of the poured concrete slurry.
Terminal Disclaimer
The terminal disclaimer filed on 12/03/2025, disclaiming the terminal portion of any patent granted on this application which would extend beyond the expiration dates of pending reference Application Number 16/48615 and of prior patent number 11440844, has been reviewed and is accepted. The terminal disclaimer has been recorded.
Accordingly, the provisional nonstatutory double patenting rejection over pending application number 16/458615 in view of Zhao et al, “Synergistic effects of silica nanoparticles/polycarboxylate superplasticizer modified graphene oxide on mechanical behavior and hydration process of cement compositions” (Zhao), and the nonstatutory double patenting rejection over US 11440884, have been withdrawn.
Response to Arguments
1) Applicant’s remarks and amendments are deemed persuasive to overcome the rejection 35 U.S.C. 112(b) rejection previously of record. Claim 7 now recites that the water to cement ratio is between about 0.400 to about 0.450 “by weight.” Although the term “by weight” is not explicitly taught in the specification, as explained in Applicant’s response and as evidenced by the attached ACI PRC-211.1-22, “Selecting Proportions for Normal-Density and High-Density Concrete-Guide,” the w/cm ratio (i.e., water/cement ratio) is known in the art as meaning the weight of water, excluding absorbed aggregate, divided by the weight of cementitious material in a mixture.” See Remarks filed 12/03/2025, pages 11-12; and ACI PRC-211.1-22; page 4, Section 3.1-“Water-cementitious materials ratio (w/cm).”
2) Applicant's arguments filed 12/03/2025, regarding the 35 USC §102(a)(1) rejection over Tian et al, CN 112408827 (Tian) have been fully considered, but they are not persuasive.
Applicant first argues:
“The prior art cited in rejecting independent claims 1 and 19 do not disclose a unique combination as claimed where the graphene admixture is in an aqueous solution that is prepared separately and independently from the pre-formed colloidal silica admixture. For at least this reason, Applicant's amended claims are patentably distinguishable over the prior art.”
Remarks, page 13.
Examiner respectfully traverses because, as stated in MPEP 2113.I:
“[E]ven though product-by-process claims are limited by and defined by the process, determination of patentability is based on the product itself. The patentability of a product does not depend on its method of production. If the product in the product-by-process claim is the same as or obvious from a product of the prior art, the claim is unpatentable even though the prior product was made by a different process." In re Thorpe, 777 F.2d 695, 698, 227 USPQ 964, 966 (Fed. Cir. 1985) (citations omitted) (Claim was directed to a novolac color developer. The process of making the developer was allowed. The difference between the inventive process and the prior art was the addition of metal oxide and carboxylic acid as separate ingredients instead of adding the more expensive pre-reacted metal carboxylate. The product-by-process claim was rejected because the end product, in both the prior art and the allowed process, ends up containing metal carboxylate. The fact that the metal carboxylate is not directly added, but is instead produced in-situ does not change the end product. (emphasis added)). Furthermore, "[b]ecause validity is determined based on the requirements of patentability, a patent is invalid if a product made by the process recited in a product-by-process claim is anticipated by or obvious from prior art products, even if those prior art products are made by different processes." Amgen Inc. v. F. Hoffmann-La Roche Ltd., 580 F.3d 1340, 1370 n. 14, 92 USPQ2d 1289, 1312, n. 14 (Fed. Cir. 2009).”
Similar to above, the presently claimed graphene admixture is initially prepared as a separate aqueous solution. The difference between the inventive product as compared to the prior art is the addition of colloidal silica and graphene as separate admixtures instead of adding a single emulsion comprising both silica and graphene. Further, there is no evidence of record to show that using separate admixtures changes the end concrete product.
3) Applicant further argues:
“Referring to Tian, the Office Action broadly states that ‘Tian teaches a recycled concrete comprising,’ inter alia, ‘nano SiO2 which is emulsified and dispersed (i.e., colloidal silica admixture).’ In other words, the Office Action takes the position that the generic teaching of nano silica dioxide in Tian is a teaching of the specific claimed colloidal silica.”
Remarks, page 13.
Examiner respectfully traverses for the following reasons. Examiner does not rely on the generic teaching of nano SiO2 particles as teaching a “colloidal silica admixture” as claimed. Instead, Examiner relies on the nano strengthening liquid of Tian, which comprises water and nano silica (Tian, page 2, lines 40-41). The nano strengthening liquid further comprises a polycarboxylate reducing agent which can fully disperse the nano materials (Tian; page 4, lines 44-45). The nano strengthening liquids are ultrasonically dispersed until it is fully emulsified and dispersed (Tian; page 3, lines 23-28 and page 5, line 48-page 6, line 27). It is the nano strengthening liquid of Tian, not the silica nano particles, that appear to be equivalent to the “colloidal silica” as claimed in that the nano silica is “fully emulsified and dispersed,” thereby suggesting a stable colloidal nano dispersion.
4) Applicant further argues:
“In Tian, the nano silica dioxide is not in the form of a colloidal suspension, as set forth in Applicant's claims. Rather, Tian repeatedly discloses that the nano silica dioxide particles (which, standing alone, are not in a colloidal suspension) are just one part of a ‘nano-strengthening liquid’ that comprises multiple elements prepared together, including GNP.”
Remarks, page 13.
Examiner respectfully traverses because the “colloidal silica admixture” as claimed does not exclude additional components due to the open “comprising” claim language. Further, as explained in 3) above, it is not the individual silica nanoparticles, but rather the fully emulsified and dispersed nano strengthening admixture of nano silica that read on the claimed “colloidal silica admixture.”
5) Applicant further argues:
“Nano silica dioxide encompasses nanoparticles in dry or aggregated forms, whereas colloidal silica is specifically limited to those nanoparticles in fluid colloidal suspension. This distinction is important because nano silica dioxide material (as in Tian) and colloidal silica (as in Applicant's claims) differ in their physical forms, states, and functional behavior within a cementitious system. The mere disclosure of nano-scale silicon dioxide particles in Tian, in dry or powder form or as unspecified particulate matter, is but one element of a multi-element "nano-strengthening liquid" and is not an affirmative teaching of silica in colloidal dispersion form standing alone, as set forth in Applicant's claims.
Remarks, pages 13-14.
This argument is not deemed persuasive for the reasons set forth in item number #3 above.
6). Applicant lastly argues:
“Persons of skill in the art understand that colloidal silica is a distinct material class characterized by discrete amorphous silica particles stably dispersed in a continuous liquid phase and typically requires specific surface chemistry, particle stabilization, and solvent-phase treatment to remain colloidally suspended.
The Tian formulation is a simple mixture of nano solids combined with a water-reducing agent, with no instruction that the nano silica dioxide is present as a pre-formed colloidal sol, nor that colloidal behavior of the pre-formed colloidal silica is necessary. Tian does not describe silica particles as being independently dispersed, surface-treated, or stabilized in a colloidal suspension, nor does it identify particle charge, sol-stability, pH control, or other properties associated with an independent colloidal sol. Tian offers no such teaching, nor any indication that its nano silica dioxide on its own possesses the aqueous dispersibility, particle stability, or amorphous sol-state characteristics of the claimed colloidal silica.”
Remarks, pages 14.
Examiner respectfully disagrees because first, the claims are directed to a concrete product comprising a colloidal silica admixture. There is no requirement that the claimed colloidal silica is a pre-formed colloidal sol (emphasis added). Second, the silica particles need not be independently present in a colloidal admixture due to the open claim language. Third, the teachings of Tian as a whole suggest that the nano silica present in the strengthening liquid are in colloidal form because: 1) they are combined with a polycarboxlic acid which would provide steric stabilization and assist with dispersion, and 2) they are dispersed using ultrasonic energy until they are fully emulsified and dispersed.
Therefore, Applicant’s Remarks have been fully considered, but are not deemed persuasive.
7). Given applicant has not provided any argument regarding the 35 U.S.C. 103 rejections of record over Adams in view of Zhao as being erroneous, the 35 U.S.C. 103 rejections of record over Adams in view of Zhao are proper and therefore maintained, as set forth on pages 9-21 above.
8). Given applicant has not provided any argument regarding the provisional nonstatutory double patenting rejection over copending Application No. 17/711,493 in view of Zhao being erroneous, and because the Terminal Disclaimer filed 12/03/2025 does not list/disclaim copending Application No. 17/711,493, the provisional nonstatutory double patenting rejection over copending Application No. 17/711,493 in view of Zhao is proper and therefore maintained as set forth on pages 23-29 above.
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.
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/CDL/Examiner, Art Unit 1732
/CORIS FUNG/Supervisory Patent Examiner, Art Unit 1732