Ex Parte Garcia-Juan et alDownload PDFPatent Trial and Appeal BoardAug 29, 201613133562 (P.T.A.B. Aug. 29, 2016) Copy Citation UNITED STA TES p A TENT AND TRADEMARK OFFICE APPLICATION NO. FILING DATE 13/133,562 06/08/2011 73673 7590 08/31/2016 Solvay America, Inc, c/o Intellectual Assets Management 3737 Buffalo Speedway Ste. 800 Houston, TX 77098-3701 FIRST NAMED INVENTOR Placido Garcia-Juan 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 ATTORNEY DOCKET NO. CONFIRMATION NO. SFG 2008/20 4025 EXAMINER KATZ, VERA ART UNIT PAPER NUMBER 1784 NOTIFICATION DATE DELIVERY MODE 08/31/2016 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): iamnafta@solvay.com tara.laposa@solvay.com PTOL-90A (Rev. 04/07) UNITED STATES PATENT AND TRADEMARK OFFICE BEFORE THE PATENT TRIAL AND APPEAL BOARD Ex parte PLACIDO GARCIA-JUAN, 1 Ulrich Seseke-Koyro, and Dagmar Bonhage Appeal2015-001747 Application 13/133,562 Technology Center 1700 Before MARK NAGUMO, KAREN M. HASTINGS, and CHRISTOPHER L. OGDEN, Administrative Patent Judges. NAGUMO, Administrative Patent Judge. DECISION ON APPEAL Placido Garcia-Juan, Ulrich Seseke-Koyro, and Dagmar Bonhage ("Garcia-Juan") timely appeal under 35 U.S.C. § 134(a) from the Final Rejection2 of claims 11, 12, and 22. 3 We have jurisdiction. 35 U.S.C. § 6. We reverse for reasons well-stated by Garcia-Juan. 1 The real party in interest is identified as Solvay Fluor GmbH. (Appeal Brief, filed 24 July 2014 ("Br."), 4.) 2 Office action mailed 21 August 2014 ("Final Rejection"; cited as "FR"), as modified by the Advisory Action mailed 31 October 2013, replacing a rejection of claims 18-21 with an objection. Appeal2015-001747 Application 13/133,562 A. Introduction4' 5 OPfNION The subject matter on appeal relates to titanium oxyfluoride (TiOF2) gels or titanyl hydroxyfluoride (TiaOb(OH)cFd, with nonstoichiometric (non- integer a, b, c, and d) compositions, as discussed infra) gels. Such gels are said to be useful for forming protective coatings on metals such as aluminum, iron, steel, and stainless steel. (Spec. 1, 11. 1-5.) These coating materials are provided as further alternatives to toxic chromium compounds widely used in the prior art. (Id. at 11. 8-17.) The '562 Specification describes the gels in the following words: Depending on the concentration of the titanium compound, the viscosity is low so that the resultant gel is pourable and can be painted, sprayed or printed onto the metal surface, or the metal parts can be dipped into the gel[.] The viscosity may be higher. The gel can even be considered as solid because it cannot be poured anymore. Often, a content of l 0 to 15 % by weight of the titanium compound is sufficient to render the gel solid. If desired, solvent can be added, and the viscosity reduced thereby; then, the resulting gel solution can be applied as described above. (Id. at 6, 11. 17-24.) 3 Claims 1-3, 5, 6, 14--17, and 23-26 have been withdrawn from consideration by the Examiner (FR 1, § 5a) and are not before us. 4 Application 13/133,562, Metals parts containing a protective coating, filed 8 June 2011 as the national stage under 35 U.S.C. § 371 of PCT/EP09/67043, filed 14 December 2009, claiming the benefit of an application filed in the EPO on 16 December 2008. We refer to the '"562 Specification," which we cite as "Spec." 5 We refer to the substitute Specification filed on 27 June 2013, although the Examiner and Garcia-Juan appear to have cited the originally filed specification. 2 Appeal2015-001747 Application 13/133,562 The gel may be in the form of a lyogel, i.e., an organic gel that "comprises the inorganic compound finely dispersed in an organic carrier." (Id. at 7, 11. 17-19.) "Alternatively," the Specification continues, "it may be used in the form of dry particles as xerogel. This means that it was produced by removing an organic solvent without changing the gel structure." (Id. at 11. 19-21; emphasis added.) General preparation of gels proceeds by treatment of titanium tetraalkoxides in a solvent (preferably alcohols, ethers, or ketones) with HF (preferably 10 to 70 % by weight in water). (Id. at 8, 11. 14--29.) If the ratio of HF to alkoxide is 2: 1 or higher, "predominantly or even only, TiOF2 is formed." (Id. at 11. 21-23.) The hydrolysis reaction is preferably performed at 30°C or higher. (Id. at 9, 11. 1-2.) Somewhat more specifically, a gel may be formed by adding a mixture of 50% HF aqueous solution and isopropyl alcohol dropwise to a stirred solution of Ti(O-i-propyl)4 in isopropanol to form a lyogel. (Spec. 16; 1. 24--14; 1. 2 (Example 4).) A xerogel is isolated "by removing the isopropanol and any other volatile constituents" (id. at 11. 3--4), more specifically, by drying overnight at 100°C (id. at 15, 11. 15-15 (Example 7)) Claim 11 is representative of the dispositive issues and reads: A titanium compound in the form of a gel, selected from the group consisting of TiOF2; TiaOb(OH)cFd wherein a is 0.8 to 1.2; bis 0.5 to 1.7; c is 0.2 to 1.7; and dis 0.2 to 1.8; and mixtures thereof. (Claims App., Br. 22; indentation, paragraphing, and emphasis added.) 3 Appeal2015-001747 Application 13/133,562 The Examiner maintains the following ground of rejection6 : Claims 11, 12, and 22 stand rejected under 35 U.S.C. § 102(b) in view of T odorova. 7 B. Discussion Findings of fact throughout this Opinion are supported by a preponderance of the evidence of record. For a reference to be anticipatory, it must describe an embodiment within the scope of the claims, i.e., an embodiment in which every limitation recited in the claim is present, and in which every relation between limitations recited or implicit in the claim is present. E.g., In re Gleave, 560 F.3d 1331, 1334 (Fed. Cir. 2009). Moreover, elements found to be present inherently must necessarily be present in or result from the prior art. In re Montgomery, 677 F.3d 1375, 1379-80 (Fed. Cir. 2012). Garcia-Juan first argues that the Examiner erred harmfully in finding that Todorova describes, based on the XPS spectrum shown in Fig. 5( c) of the TF20 sample calcined at 400°C, the presence of a TiOF2 xerogel. (Br. 8-17.) Second, Garcia-Juan argues that there is no disclosure or evidence supporting the finding that Todorova prepares TiOF2 or other titanium oxyfluorides; instead, Garcia-Juan argues, Todorova more likely prepares a titanium salt of fluoroacetic acid. (Br. 17-19.) The weight of the evidence supports Garcia-Juan's arguments. 6 Examiner's Answer mailed 16 September 2014 ("Ans."). 7 N. Toderova et al., Preparation of fluorine-doped Ti02 photocatalysts with controlled crystalline structure, Int'l. J. Photoenergy, Article ID 534038, doi: 10.1155/2008/534038 (2008). 4 Appeal2015-001747 Application 13/133,562 Todorova prepares fluorine-doped Ti02 powders by adding tetraethyl orthotitanate (TEOTi, Ti(-OCH2CH3)4) dropwise to solutions of fluoroacetic acid (CF3COOH) in water (molar ratio of H20:TEOTi = 18), stirring at room temperature for 24 hours, and then air-drying at 90°C to yield xerogels. (Todorova 2, col. 1, Experimental.) The as-prepared xerogels were calcined at 400°C to 600°C to yield powders. The crystalline structure of the powders was investigated by X-ray diffraction (XRD). According to Table 1 (id. at 4; not reproduced here), the phase content of the powder was about 9% anatase and 91 % rutile at 400°C, and 100% rutile at 500°C and at 600°C. The chemical state of the elements in the powder samples were evaluated by X-ray photoelectron spectroscopy (XPS). In the words of Todorova, "[t]he spectra obtained for Ti 2p, 0 ls, and F ls regions (Figure 5) revealed that the powder consists of Ti02, where titanium and oxygen are present as Ti4+ and 0 2-." (Id. at 6, 1st fhll para.) Figure 5(c), reproduced below, {Todorova Fig. 5c shows the F 1 s XPS spectrum of sample TF20; added lines show approximate positions of 684.3 e V, 685.4 e V, and 688 e V} 5 Appeal2015-001747 Application 13/133,562 shows the F ls region of the XPS spectra of TF20 (FIT= 20/80 atomic ratio (id.)). According to Todorova, The F ls spectrum (Figure 5(c)) is nonsymmetric and the contribution near 684.3 e V indicates that the fluorine is presented in the sample mainly as TiF4 and/or to physically adsorbed F- on Ti02. The contribution near 685.4 e V could be related to TiOF2 structures and the tail near 688 eV to nonstoichiometric solid solution of Fin Ti02 of the Ti02-xFx type. It can be also associated with C-F bonding in CF3 residual groups. (Id.; footnotes omitted, emphasis added.) The Examiner does not direct our attention to any indication in this passage, beyond the possible presence of TiOF2 itself, that the TiOF2 is present as a gel. The possibility that the contribution to the peak intensity near 685.4 e V may be due to TiOF2 does not suffice to demonstrate the inherent presence of TiOF2, nor does it show that TiOF2 is present as a gel. The rejection for anticipation falls for this reason alone. Similarly, the weight of the evidence is against the Examiner's conclusion that because the xerogel was calcined, the burden is on Garcia-Juan to show that the calcined sample does not contain a gel. As Garcia-Juan urges, the description of the thermogravimetric (TG) and differential thermal analysis (DT A) data shown in Figure 1 (not reproduced here) indicates that the mass decrease of the samples occurs in three stages. Todorova interprets the second stage of mass decrease as being "connected to the decomposition and removal of 6 Appeal2015-001747 Application 13/133,562 organic radicals (CF 3COO-)." (Todorova 3, col. I. 8) This decomposition and removal of organic radicals that did not arise from solvent appear to be inconsistent with the definition provided by the '562 Specification that a xerogel is produced from a lyogel "by removing an organic solvent without changing the gel structure" (Spec. 7, 11. 1-21, emphasis added). The Examiner has not come forward with any credible evidence or argument indicating that Todorova's interpretation should be disregarded. Moreover, although Garcia-Juan does not support its speculation that the process reported by T odorova results in the formation of titanium salts of fluoroacetic acid (Br. 18, 11. 1-9), we note that the Examiner has not explained why the rather different reaction conditions reported by Todorova (TEOTi solution dripped into aqueous fluoroacetic acid) would have been expected to result in the same product reported by Garcia-Juan (HF aqueous solution dripped into solutions of titanium alkoxide ). We conclude that Garcia-Juan has shown harmful error in the rejection for anticipation based on Todorova. C. Order It is ORDERED that the rejection of claims 11, 12, and 22 is reversed. REVERSED 8 Although the quoted language refers to the TFIO sample, Todorova reports that the thermal behavior of TF20 xerogel (not given) was similar to the TFIO sample." (Todorova 3, 1st col.) 7 Copy with citationCopy as parenthetical citation