Ex Parte Zhamu et alDownload PDFBoard of Patent Appeals and InterferencesJul 18, 201211879680 (B.P.A.I. Jul. 18, 2012) Copy Citation UNITED STATES PATENT AND TRADEMARKOFFICE UNITED STATES DEPARTMENT OF COMMERCE United States Patent and Trademark Office Address: COMMISSIONER FOR PATENTS P.O. Box 1450 Alexandria, Virginia 22313-1450 www.uspto.gov APPLICATION NO. FILING DATE FIRST NAMED INVENTOR ATTORNEY DOCKET NO. CONFIRMATION NO. 11/879,680 07/19/2007 Aruna Zhamu 4616 7590 07/18/2012 Bor Z. Jang 9436 Parkside Drive Centerville, OH 45458 EXAMINER LEE, REBECCA Y ART UNIT PAPER NUMBER 1734 MAIL DATE DELIVERY MODE 07/18/2012 PAPER Please find below and/or attached an Office communication concerning this application or proceeding. The time period for reply, if any, is set in the attached communication. PTOL-90A (Rev. 04/07) UNITED STATES PATENT AND TRADEMARK OFFICE ____________ BEFORE THE BOARD OF PATENT APPEALS AND INTERFERENCES ____________ Ex parte ARUNA ZHAMU, JINJUN SHI, JOAN JANG, and BOR Z. JANG __________ Appeal 2011-002839 Application 11/879,680 Technology Center 1700 ____________ Before ADRIENE LEPIANE HANLON, TERRY J. OWENS, and MICHAEL P. COLAIANNI, Administrative Patent Judges. COLAIANNI, Administrative Patent Judge. DECISION ON APPEAL Appeal 2011-002839 Application 11/879,680 2 Appellants appeal under 35 U.S.C. § 134 the final rejection of claims 1-20, 23-26, and 29-42. We have jurisdiction over the appeal pursuant to 35 U.S.C. § 6(b). We AFFIRM. Appellants’ invention is directed to a method of exfoliating and separating graphite, graphite oxide and other laminar compounds to produce nano-scaled platelets, particularly nano-scaled graphene platelets (NGPs) with an average thickness of no more than 2 nm or 5 layers (i.e., 5 graphene sheets) (Spec. 1:14-17). Claim 1 is illustrative: 1. A method of producing ultra-thin, separated nano- scaled platelets from a layered graphite material, said method comprising: a) using a method involving no alkali metal intercalation to provide a supply of nano-scaled graphite platelets or exfoliated graphite flakes with an average platelet or flake thickness of no more than 10 nm or, on an average, having no more than 30 layers per platelet or flake; and b) intercalating said supply of nano-scaled platelets or exfoliated flakes to produce intercalated nano platelets or flakes containing no alkali intercalant and exfoliating said intercalated nano platelets or flakes at a temperature and a pressure for a sufficient period of time to produce said ultra-thin nano-scaled platelets having an average thickness less than 2 nm or comprising, on an average, no more than 5 layers per platelet. Appeal 2011-002839 Application 11/879,680 3 Appellants appeal the following rejections1: 1. Claims 1-10, 24, 25, 29, and 38-42 are rejected under 35 U.S.C. § 103(a) as being unpatentable over Viculis (Lisa M. Viculis et al., Intercalation and Exfoliation Routes to Graphite Nanoplatelets, 15 J. MATERIALS CHEMISTRY 974 (2005)) in view of Mack (Julia J. Mack et al., Graphite Nanopatelet Reinforcement of Electrospun Polyacrylonitrile Nanofibers, 17 ADVANCED MATERIALS 77 (2005)) and Chen (Guohua Chen et al., Preparation and Characterization of Graphite Nanosheets from Ultrasonic Powdering Technique, 42 CARBON 753 (2004)). 2. Claims 11-18, 23, 26, and 30 are rejected under 35 U.S.C. § 103(a) as being unpatentable over Bunnell (US 5,186,919 issued Feb. 16, 1993) in view of Mack. 3. Claims 19 and 20 are rejected under 35 U.S.C. § 103(a) as being unpatentable over Bunnell in view of Mack and Lu (Wei Lu et al., Epoxy Resin/Graphite Electrically Conductive Nanosheet Nanocomposite, 21 MATERIALS & MANUFACTURING PROCESSES 167 (2006)). 4. Claims 31-37 are rejected under 35 U.S.C. § 103(a) as being unpatentable over Bunnell. 1 Appellants do not list the provisional obviousness-type double patenting rejection of claims 11-15 and 17-20 over claims 1-10 of copending application 11/807,728 as being on appeal though the Examiner maintains the rejection (App. Br. 9, 17-18; Ans. 14-15). Application 11/807,728 issued as U.S. Patent 7,497,205. We summarily affirm this rejection of the Examiner, as it has not been contested by Appellants. Appeal 2011-002839 Application 11/879,680 4 5. Claims 1, 2, 8, 24, and 25 are provisionally rejected on the ground of nonstatutory obviousness-type double patenting as being unpatentable over claims 1, 2, 4, 10, and 12 of application 11/881,389. 6. Claims 1, 2 and 8 are provisionally rejected on the ground of nonstatutory obviousness-type double patenting over claims 1, 3, 5, 8, 14, and 15 of copending application 11/787,442. REJECTION (1) Appellants’ arguments focus on claims 1 and 29 (App. Br. 10-15). We note that Appellants’ arguments regarding claims 11, 30, 31, and 37 are not germane to any of the rejections as these claims have not be included in rejection (1) and Viculis has not been included in any other rejection where claims 11, 30, 31, and 37 were rejected (App. Br. 12-13, 14; Ans. 4-8). ISSUE Did the Examiner reversibly err in determining that the combined teachings of Viculis, Mack and Chen would have suggested the subject matter of claims 1 and 29? We decide this issue in the negative. FINDINGS OF FACT AND ANALYSES The Examiner finds that Viculis teaches the subject matter of claim 1, except for the supply of nano-scaled platelets or exfoliated flakes have an average platelet or flake thickness of no more than 10 nm or, on average, having no more than 30 layers per platelet or flake and no use of alkali metal intercalants (Ans. 4-5). The Examiner finds that Mack teaches exfoliated nanoplatelets having a thickness of 40 ± 15 layers, which would include Appeal 2011-002839 Application 11/879,680 5 platelets with a thickness of 25 layers (id. at 5). The Examiner finds that Chen teaches acid used as an intercalant to produce nanoscaled graphite platelets (id.). The Examiner concludes that it would have been obvious to use Mack’s exfoliated platelets as the starting material in order to provide a starting material required by Viculis’ process (id.). The Examiner further concludes that using Chen’s acid as an intercalant in lieu of Viculis’ alkali metal intercalant would have been obvious because the applied prior art teaches the acid or alkali metal intercalant are functional equivalents (id.). Appellants argue that Viculis does not teach or suggest the reintercalation of the exfoliated particles to achieve exfoliated nano-scaled platelets having an average thickness of less than 2 nm (App. Br. 10-11). Appellants contend that the argued documentary evidence on pages 11-12 of the Brief establishes that the skilled artisans did not appreciate Appellants’ claimed reintercalation-reexfoliation process until two years after Appellants’ filing date which emphasizes the novelty and non-obviousness of the claimed method. Id. at 12. Appellants’ argument is contradicted by the Viculis reference that teaches the reintercalation of exfoliated graphite: Here we describe how graphite that has already been intercalated with oxidizing acids and exfoliated by rapid heating can be improved. The exfoliated graphite is reintercalated with alkali metals and exfoliated with aqueous solvents to produce even thinner platelets than previously reported, on the order of 2-150 nm in thickness. Viculis 974. Thus, Viculis teaches reintercalation of exfoliated graphite. Though Appellants contend that Viculis does not teach achieving a graphite sheet having a thickness of less than 2 nm (App. Br. 11, 13-14), Appellants do not specifically respond to the Examiner’s finding that Appeal 2011-002839 Application 11/879,680 6 Viculis’ teaching of forming a graphite sheet with a thickness in the range of 2-150 nm is close enough to Appellants’ claimed 2 nm or less range to expect Viculis’ graphite sheet to have the same property (Ans. 42). While Appellants contend that thinner nano-graphene platelets (NGP) have fundamentally different properties than thicker NGP (App. Br. 15), Appellants do not refer us to any objective evidence that shows that Viculis’ teaching of a 2 nm thick graphite sheet would not be reasonably expected to have the same properties as a slightly less than 2 nm thick graphite sheet as found by the Examiner. The evidence contained in the Evidence Appendix of the Brief merely shows the thickness of the graphite sheets achieved with different intercalants; it does not establish any difference in property as argued. Appellants further argue that Chen’s teaching to use acid as an intercalant does not add support to the combination of Viculis and Mack because Viculis teaches using acid as the intercalant for the initial intercalation and exfoliation step (App. Br. 13). Appellants contend that Viculis reintercalates with alkali metal, which as shown by the evidence reproduced from the August 11, 2009 response presented in the Evidence Appendix, produces thicker graphite sheets (id. at 13-14). These arguments are unpersuasive because they fail to address the Examiner’s finding that Chen, Viculis and Mack teach that acid and alkali metal are functionally equivalent intercalants (Ans. 5). Based on this functional equivalency of the intercalants, the Examiner concludes that it would have been obvious to substitute an acid for Viculis’ alkali metal 2 The Examiner refers to the Manual of Patent Examining Procedure (MPEP) § 2144.05(I), which relies on Titanium Metals Corp. of Am. v. Banner, 778 F.2d 775 (Fed. Cir. 1985) to support the Examiner’s position. Appeal 2011-002839 Application 11/879,680 7 intercalant with expected success. Id. See In re Fout, 675 F.2d 297, 301 (CCPA 1982) (“Express suggestion to substitute one equivalent for another need not be present to render such substitution obvious.â€). Moreover, Appellants’ argument that the proffered evidence shows that alkali metal intercalants always produce thicker graphite sheets is undermined by Viculis’ teaching that the resulting thickness of the graphite sheets may be 2 nm as the lower end of the range. As noted above, the Examiner finds and Appellants do not dispute that this Viculis graphite sheet thickness disclosure is close enough to the claimed graphite sheet thickness range (i.e., 2 nm or less) that it would have been reasonable to expect that the graphite sheets have the same property. Appellants argue that Mack only teaches an average thickness of the graphite sheet being between 40 ± 15 layers, which is different than Appellants’ claimed average thickness of no more than 30 layers (App. Br. 14). Appellants contend that most of Mack’s graphite sheets would have a thickness greater than the claimed thickness. Id. Contrary to Appellants’ arguments, the fact that Mack’s graphite sheet thickness range overlaps the claimed graphite sheet thickness range would have rendered the claimed range prima facie obvious. In re Peterson, 315 F.3d 1325, 1329 (Fed. Cir. 2003). Regarding claim 29, Appellants argue that Mack does not teach the more narrowly claimed graphite sheet thickness range (i.e., 24 layers or less per platelet) (App. Br. 14). However, the Examiner finds that Mack’s range (i.e., 25 to 55 layers) is so close to Appellants’ claim 29 range of graphite thicknesses, the two materials are reasonably expected to have the same Appeal 2011-002839 Application 11/879,680 8 property (Ans. 8). Appellants do not respond to or address the Examiner’s specific findings and treatment of claim 29. Finally, Appellants argue that there is no reason absent hindsight to use Mack’s exfoliated graphite as the starting material in Viculis’ process (App. Br. 14-15). However, the Examiner reasons that one of ordinary skill in the art would have been motivated to do so to provide a starting material to Viculis’ process (Ans. 5). In other words, the reason for using Mack’s exfoliated graphite as the initial exfoliated graphite in Viculis’ process stems from Viculis’ use of exfoliated graphite as the starting material and the knowledge of one skilled in the art. We do not find that the Examiner engaged in impermissible hindsight in reaching this conclusion. For the above reasons, we affirm the Examiner’s § 103 rejection over Viculis in view of Mack and Chen. REJECTIONS (2) to (4) Appellants’ arguments focus on claim 11 of rejection (2) only (App. Br. 16). Regarding rejections (3) and (4), Appellants rely on arguments made regarding claim 11 under rejection (2) (id. at 16-17). Accordingly, claims 19, 20, and 31-37 will stand or fall with our analysis regarding claim 11 under rejection (2). ISSUE Did the Examiner reversibly err in finding that Bunnell teaches the same ultrasonication step as claimed such that one of ordinary skill in the art would have expected the ultrasonication step of Bunnell to be able to Appeal 2011-002839 Application 11/879,680 9 perform the same function (i.e., exfoliation) as claimed? We decide this issue in the negative. FINDINGS OF FACT & ANALYSIS The Examiner finds that Bunnell teaches all the steps recited in claim 11 including the use of ultrasonication to exfoliate nano-graphene platelets (Ans. 8). The Examiner further finds that Bunnell teaches the same ultrasonication step as claimed such that one of ordinary skill in the art would have expected the ultrasonication step of Bunnell to perform the same function as claimed (id. at 16). Appellants argue that Bunnell does not teach using ultrasonication to exfoliate, but rather uses ultrasonication merely to break-up the previously exfoliated product (App. Br. 16). Claim 11 requires that the steps of providing a supply of nano-scaled graphite platelets or exfoliated graphite flakes, dispersing the supply of nano-scaled platelets or flakes in a liquid medium containing a surfactant to form a suspension, and exposing the suspension to direct ultrasonication at a sufficient energy level and time to exfoliate and separate the ultra-thin nano- scaled platelets into having an average thickness of less than 2 nm or comprising, on an average, no more than 5 layers per platelet (Claim App’x). Appellants disclose that the ultrasonication power is usually greater than 80 Watts, with a preference for higher energy level to exfoliate (Spec. 8:2; 16:11-13). Appellants exemplify ultrasonication at 125 W for 1 hour (id. at 18, Ex. 2 and 3). Appellants preface the exemplary disclosure by stating that these disclosures do not limit the scope of the invention (Spec. 17:17-18). Appeal 2011-002839 Application 11/879,680 10 Bunnell teaches providing exfoliated graphite sheets, adding hexane and fish oil as a surfactant and then ultrasonicating for five minutes at 345 W (col. 4, Ex. A). Based on these disclosures, Appellants’ arguments fail to persuade us of any patentable distinction between Bunnell’s disclosure and Appellants’ claimed invention. Rather, we agree with the Examiner that Bunnell teaches the same step of ultrasonication of a dispersed, exfoliated graphite material. Bunnell teaches that the ultrasonication is performed at an energy level (i.e., 345 W) within Appellants’ disclosed range (i.e., greater than 80 Watts). Accordingly, though not specifically disclosed by Bunnell, it would have been reasonably expected that exfoliation would have occurred during Bunnell’s ultrasonication process. The Examiner has established a prima facie case of obviousness such that the burden shifted to Appellants to show nonobviousness. Appellants’ mere argument that Bunnell fails to teach that exfoliation occurs during the ultrasonication step fails to satisfy their burden. The preponderance of the evidence favors the Examiner’s obviousness conclusion. We affirm the Examiner’s rejections (2) to (4). REJECTIONS (5) AND (6) We note that application 11/881,389 used in the Examiner’s provisional obviousness-type double patenting rejection (5) was abandoned on May 24, 2011. Accordingly, rejection (5) is moot. Regarding rejection (6), application 11/787,442 issued as US Patent 8,132,746. Appellants argue that the Examiner’s only justification for the rejection is based upon the application involving processes in which nano- Appeal 2011-002839 Application 11/879,680 11 graphene platelets are produced by a combination of intercalation and exfoliation steps without accounting for the specific and distinctly different steps of the claimed processes (App. Br. 17). We have reviewed the Examiner’s rejection on page 14 of the Answer and agree with Appellants that the Examiner has not satisfied the burden of establishing a prima facie case of unpatentability. The Examiner has not made specific findings regarding the differences between the claimed processes and resolved why the differences would have been obvious. Contrary to the Examiner’s argument that Appellants have not specifically pointed out the differences between the claimed inventions, it is the Examiner’s initial burden to point out the differences between the claimed inventions in making the prima facie case. For these reasons, we reverse the Examiner’s nonstatutory obviousness-type double patenting rejection over application 11/787,442, now US Patent 8,132,746. DECISION The Examiner’s decision is affirmed. No time period for taking any subsequent action in connection with this appeal may be extended under 37 C.F.R. § 1.136. ORDER AFFIRMED bar Copy with citationCopy as parenthetical citation