UChicago Argonne, LLCDownload PDFPatent Trials and Appeals BoardJul 16, 20202019004840 (P.T.A.B. Jul. 16, 2020) Copy Citation UNITED STATES PATENT AND TRADEMARK OFFICE 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. 15/006,456 01/26/2016 Guiliang Xu 051583-0698 9154 23524 7590 07/16/2020 FOLEY & LARDNER LLP 3000 K STREET N.W. SUITE 600 WASHINGTON, DC 20007-5109 EXAMINER SIDDIQUEE, MUHAMMAD S ART UNIT PAPER NUMBER 1723 NOTIFICATION DATE DELIVERY MODE 07/16/2020 ELECTRONIC 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. Notice of the Office communication was sent electronically on above-indicated "Notification Date" to the following e-mail address(es): ipdocketing@foley.com PTOL-90A (Rev. 04/07) UNITED STATES PATENT AND TRADEMARK OFFICE BEFORE THE PATENT TRIAL AND APPEAL BOARD Ex parte GUILIANG XU, ZONGHAI CHEN, and KHALIL AMINE Appeal 2019-004840 Application 15/006,456 Technology Center 1700 Before JEFFREY T. SMITH, LINDA M. GAUDETTE, and MERRELL C. CASHION, JR., Administrative Patent Judges. GAUDETTE, Administrative Patent Judge. DECISION ON APPEAL1 The Appellant2 appeals under 35 U.S.C. § 134(a) from the Examiner’s decision finally rejecting claims 1–11, 13–16, and 18–20.3 We AFFIRM. 1 This Decision includes citations to the following documents: Specification filed January 26, 2016 (“Spec.”); Final Office Action dated July 20, 2018 (“Final”); Appeal Brief filed January 23, 2019 (“Appeal Br.”); Examiner’s Answer dated April 12, 2019 (“Ans.”); and Reply Brief filed June 3, 2019 (“Reply Br.”). 2 We use the word “Appellant” to refer to “applicant” as defined in 37 C.F.R. § 1.42. The Appellant identifies the real party in interest as UChicago Argonne LLC. Appeal Br. 1. 3 We have jurisdiction under 35 U.S.C. § 6(b). Appeal 2019-004840 Application 15/006,456 2 CLAIMED SUBJECT MATTER The invention relates to phosphorus-carbon composites that can be used as battery anode materials. Claims 11 and 16, reproduced below from the Appeal Brief Claims Appendix, are illustrative of the claimed subject matter: 11. A phosphorus-carbon composite comprising conductive carbon matrix and nano-sized phosphorus particles, wherein: the nano-sized phosphorus particles comprise black phosphorus; the nano-sized phosphorus particles are uniformly dispersed on the surface and/or pores of the carbon matrix; and the carbon matrix comprises: one or more of graphite, graphene, expanded graphite, reduced graphene oxide, acetylene black, carbon black, a metal-organic framework, porous carbon, carbon spheres, or carbon aerogel; and one or more of single-walled carbon nanotubes, multi-walled carbon nanotubes, carbon nanofibers, carbon nanotube arrays, polypyrrole, or polyaniline. 16. A method to prepare the phosphorus-carbon composite of claim 11, the method comprising ball milling a mixture comprising two or more precursors for the conductive carbon matrix; and phosphorus. Appeal 2019-004840 Application 15/006,456 3 REFERENCES The Examiner relies on the following prior art as evidence of unpatentability: Name Reference Date Park Wang Kim Tour Hahn US 2008/0038626 A1 US 2013/0224369 A1 US 2016/0301103 A1 US 2016/0379764 A1 US 2017/0092439 A1 Feb. 14, 2008 Aug. 29, 2013 Oct. 13, 2016 Dec. 29, 2016 Mar. 30, 2017 REJECTIONS 1. Claims 1, 9, 11, 13–16, and 18–20 are rejected under 35 U.S.C. § 103 as unpatentable over Park in view of Wang and Hahn. 2. Claims 2–7 are rejected under 35 U.S.C. § 103 as unpatentable over Park in view of Wang, Hahn and Tour. 3. Claims 8 and 10 are rejected under 35 U.S.C. § 103 as unpatentable over Park in view of Wang, Hahn, Tour, and Kim. OPINION The Examiner found that “Park discloses a battery comprising an anode wherein the anode comprises . . . a black phosphorus-carbon composite material.” Final 3. The Examiner acknowledged that “Park [is] silent about nano-sized phosphorous particles and the carbon matrix as claimed.” Id. The Examiner found, however, that one of ordinary skill in the art would have included these features in Park’s anode based on Wang’s and Hahn’s disclosures. See id. at 3–5; e.g., id. at 5 (noting that “the substitution of one known element for another would have yielded predictable results to one of ordinary skill in the art at the time of the invention”). More specifically, the Examiner found that “Wang discloses a battery comprising Appeal 2019-004840 Application 15/006,456 4 an anode wherein the anode comprises . . . phosphorus uniformly deposited and adsorbed in [a] plurality of micropores of the porous conductive carbon material,” and the phosphorus particles have diameters ranging from about 10 nanometers to about 100 micrometers. Id. at 3–4. The Examiner found that “Hahn teaches an electrochemical cell wherein the carbon in the composite material . . . of the anode is preferably in a polymorph selected from the group consisting of carbon nanotubes, carbon nanofibers, graphene, functionalized graphene, activated carbon, and mixtures thereof.” Id. at 4–5. As to the rejection of claims 1, 9, 11, 13–16, and 18–20, the Appellant contends that the Examiner reversibly erred in rejecting the claims because: “(1) modification of the cited prior art would render it unsatisfactory for its intended use; (2) [the] combination of the cited prior art fails to provide the required expectation of success; and (3) the conclusions of obviousness were made through impermissible hindsight.” Appeal Br. 5; see generally id. at 7– 11. The Appellant also argues separately in support of patentability of claim 16, contending that the applied prior art fails to teach or suggest “a mixture comprising two or more precursors for the conductive carbon matrix.” Id. at 11–12. We agree with the Examiner that these arguments are not persuasive of reversible error essentially for the reasons explained in the Answer. See generally Ans. 6–10. We add the following primarily to address the arguments made in the Appellant’s Reply Brief. The Appellant argues that Park produces a black phosphorus-carbon composite through high energy ball-milling of a mixture of red phosphorus and carbon-based powder. Appeal Br. 7. The Appellant argues that Wang produces a red phosphorus composite by subliming and condensing red phosphorus onto a porous, conductive, carbon material (id.), and that “[t]he Appeal 2019-004840 Application 15/006,456 5 property of nano-sized phosphorus particles . . . is conferred by the sublimation-condensation process itself” (Reply Br. 2). The Appellant argues that “[t]he Examiner provides no rationale as to how one of ordinary skill in the art would modify Park to incorporate Wang's teaching of nano- sized phosphorus particles,” and the Examiner has not shown that the ordinary artisan would have had a reasonable expectation of success in obtaining nano-sized, black, phosphorus particles using Park’s ball-milling process. Id. at 3–4. We are not persuaded that the Examiner failed to meet the initial burden to establish a prima facie case of obviousness. As explained in the Answer, and acknowledged by the Appellant, the Examiner relied on Wang for a teaching that “it is well known in the art that utilizing nanoparticles of active materials can exhibit improved performance in energy storage devices compared to traditional electrodes that do not take advantage of nanomaterials.” Ans. 7; see Reply Br. 2. However, a finding that the ordinary artisan would have modified Park’s phosphorus-carbon composite to include nano-sized phosphorus particles was unnecessary to support a conclusion of obviousness. See Reply Br. 5 (arguing that “one of ordinary skill in the art would not be motivated to look to Wang’s teachings and modify Park based on Wang’s process”). As found by the Examiner (see Ans. 8), in preparing the composite, Park uses process conditions similar to those used by the Appellant and, therefore, Park’s method would have been expected to produce a composite comprising nano-sized particles. Compare Spec. ¶¶ 55–57 (“The ball milling may be performed at a rotation speed of about 300 to about 1500 rpm. . . . In some embodiments, the rotation speed is about 300 [or] . . . 600 . . . . The ball milling may be performed for a time period of about 1 to about 40 hours. . . . This includes a time period of . . . Appeal 2019-004840 Application 15/006,456 6 about 10 to about 15 hours . . . under inert atmosphere (e.g., argon gas) . . . .”), id. ¶ 14, Figure 1 (describing a high energy ball milling process using stainless steel balls) and id. ¶ 73 (Example 1: “The weight ratio of the balls and the mixture was maintained in a ratio of 10.”), with Park ¶ 28 (“The prepared mixture is put into the cylindrical vial with a ball and then the mechanical synthesis is carried out with a rotation velocity of 300 times or more per minute using the general high energy ball-milling devices . . . . The exemplary ratio of the ball to the powder is 16–24:1 . . . .”) and id. ¶ 37 (“Then, the mixture and stainless steel ball . . . were put into a hardened steel cylindrical vial . . . and the HEMM [(high energy mechanical milling (id. ¶ 22))] process was conducted with a rotation velocity of 600 times per minute under an Ar atmosphere in a glove box for 12 hours . . . .”). Park and the Appellant also describe similar starting materials. Compare Spec ¶ 6 (“[T]he nano-sized phosphorus particles include black phosphorus, red phosphorus, or any combination thereof), ¶ 80 (“[T]he particle size of bulk black phosphorus is about hundreds of micrometers.”) and ¶ 42 (“The conductive carbon matrix may include, but is not limited to, graphite, . . . acetylene black, carbon black, . . . carbon nanotubes, . . . polypyrrole, polyaniline, and mixtures of any two or more such materials.”), with Park ¶ 37 (exemplary preparation of black phosphorus-carbon composite using “[c]ommercially available Red Phosphorus powder . . . average size: 75 μm”) and ¶ 25 (listing exemplary carbon-based powders including acetylene black, carbon black, and graphite carbon). When an examiner demonstrates that a claimed process appears to be identical to a prior art process or that the claimed and prior art products appear to be the same, the burden is properly shifted to the applicant to show Appeal 2019-004840 Application 15/006,456 7 that they are not. See In re Spada, 911 F.2d 705, 708 (Fed. Cir. 1990); In re Best, 562 F.2d 1252, 1254–56 (CCPA 1977). The Appellant has not made persuasive arguments or identified sufficient objective evidence to meet this burden. The Appellant argues that Park’s and the Appellant’s process conditions differ because “the Appellant explicitly teaches in Example 1 that ball milling is conducted at 1425 rpm for 700 minutes, conditions that are higher in ball milling speed and duration and not similar to Park’s conditions.” Reply Br. 5. The Specification disclosure cited in the comparisons with Park’s disclosure, above, however, does not support a finding that the specific Example 1 process conditions are necessary to produce the claimed nano-sized phosphorus particles. The Appellant also argues that the Examiner’s statement that “[t]here are plenty of teachings in the prior art where high energy ball-milling is used to make nanoparticles” “amounts to improper Official Notice” because the Examiner did not provide proper citation. Reply Br. 7. This finding is unnecessary to establish a prima facie case of obviousness for the reasons discussed above. Accordingly, because we do not rely on this finding, we decline to consider the Appellant’s argument that “the Examiner's Answer has failed to satisfy its obligations under MPEP § 2144.03” (Reply Br. 7). In the Appeal Brief, the Appellant argues that Hahn fails to provide any guidance to use a dual-component conductive carbon matrix as claimed in each of independent claims 1, 9, and 11, or “a method comprising ball milling a mixture comprising two or more precursors for the conductive carbon matrix; and phosphorus” as recited in claim 16. Appeal Br. 9, 11–12. The Examiner has fully addressed these arguments and explained why they Appeal 2019-004840 Application 15/006,456 8 are not persuasive. See Ans. 8–11. We additionally note that Wang, like Hahn, discloses that the carbon matrix components are selected from a limited list that includes materials from both of the groups recited in the independent claims: “the porous conductive carbon material is selected from the group consisting of porous carbon, charcoal, carbon black, mesophase carbon micro beads, hollow carbon fiber, carbon nanotubes with open ends, and combinations thereof” (Wang claim 5 (emphasis added)). As to claim 16, the Appellant has not addressed the Examiner’s finding that Wang discloses ball milling a mixture comprising porous carbon powders and phosphorus (Final 5 (citing Wang ¶ 54)). See Appeal Br. 11–12. In sum, for the reasons stated above and in the Answer, the Appellant has not convinced us of reversible error in the Examiner’s rejection of claims 1, 9, 11, 13–16, and 18–20 over Park in view of Wang and Hahn. We turn next to the rejection of claims 2–7 over Park in view of Wang, Hahn and Tour. Each of dependent claims 2–7 recites that the claim 1 electrochemical device comprises a specific type of battery: sodium-ion (claims 2, 7), zinc-ion (claim 3), calcium-ion (claim 4), magnesium-ion (claim 5), and aluminum-ion (claim 6). The Examiner found that “Park/Wang teaches a lithium ion battery” and Tour teaches that “it [was] known in the art to utilize similar material[s]/technique[s] in . . . similar electrochemical device[s].” Final 5–6. The Appellant argues that there is no “teaching or suggestion that simply because Tour’s nickel hydroxide nanoporous film electrodes may be use[d] in numerous battery types, then the instantly claimed phosphorus-carbon composite may also be used in numerous battery types as claimed.” Appeal Br. 10. Appeal 2019-004840 Application 15/006,456 9 The Appellant’s argument is not persuasive of reversible error because the Appellant has not explained why it was erroneous or unreasonable for the Examiner to find that Tour’s batteries, as well as the claimed batteries, would have been expected to work in similar manner because they are all metal-ion batteries. See Ans. 9. We add that in addition to teaching a lithium ion battery, Park explicitly states that the “black phosphorus-carbon composite also can be applied to other kinds of rechargeable batteries such as Magnesium rechargeable batteries etc.” Park ¶ 48. In sum, the Appellant has not convinced us of reversible error in the Examiner’s rejection of claims 2–7 over Park in view of Wang, Hahn, and Tour for the reasons stated above and in the Answer. As to the rejection of claims 8 and 10 over Park in view of Wang, Hahn, Tour, and Kim, the Examiner has fully addressed the Appellant’s arguments and we are not persuaded of reversible error for the reasons stated in the Answer. See Ans. 10. DECISION SUMMARY Claims Rejected 35 U.S.C. § Reference(s)/Basis Affirmed Reversed 1, 9, 11, 13–16, 18–20 103 Park, Wang, Hahn 1, 9, 11, 13–16, 18–20 2–7 103 Park, Wang, Hahn, Tour 2–7 8, 10 103 Park, Wang, Hahn, Tour, Kim 8, 10 Overall Outcome: 1–11, 13– 16, 18–20 Appeal 2019-004840 Application 15/006,456 10 TIME PERIOD FOR RESPONSE No time period for taking any subsequent action in connection with this appeal may be extended under 37 C.F.R. § 1.136(a). AFFIRMED Copy with citationCopy as parenthetical citation