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WO 2013/109674 Al 25 July 2013 (25.07.2013) P O P C T

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WO 2013/109674 Al 25 July 2013 (25.07.2013) P O P C T (12) INTERNATIONAL APPLICATION PUBLISHED UNDER THE PATENT COOPERATION TREATY (PCT) (19) World Intellectual Property Organization I International Bureau (10) International Publication Number (43) International Publication Date WO 2013/109674 Al 25 July 2013 (25.07.2013) P O P C T (51) International Patent Classification: (81) Designated States (unless otherwise indicated, for every C03C 17/30 (2006.01) B44C 1/00 (2006.01) kind of national protection available): AE, AG, AL, AM, C03C 21/00 (2006.01) AO, AT, AU, AZ, BA, BB, BG, BH, BN, BR, BW, BY, BZ, CA, CH, CL, CN, CO, CR, CU, CZ, DE, DK, DM, (21) Number: International Application DO, DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, GT, PCT/US2013/021815 HN, HR, HU, ID, IL, IN, IS, JP, KE, KG, KM, KN, KP, (22) International Filing Date: KR, KZ, LA, LC, LK, LR, LS, LT, LU, LY, MA, MD, 17 January 2013 (17.01 .2013) ME, MG, MK, MN, MW, MX, MY, MZ, NA, NG, NI, NO, NZ, OM, PA, PE, PG, PH, PL, PT, QA, RO, RS, RU, (25) Filing Language: English RW, SC, SD, SE, SG, SK, SL, SM, ST, SV, SY, TH, TJ, (26) Publication Language: English TM, TN, TR, TT, TZ, UA, UG, US, UZ, VC, VN, ZA, ZM, ZW. (30) Priority Data: 12305068.4 19 January 2012 (19.01.2012) EP (84) Designated States (unless otherwise indicated, for every kind of regional protection available): ARIPO (BW, GH, (71) Applicant: CORNING INCORPORATED [US/US]; 1 GM, KE, LR, LS, MW, MZ, NA, RW, SD, SL, SZ, TZ, Riverfront Plaza, Corning, New York 1483 1 (US). UG, ZM, ZW), Eurasian (AM, AZ, BY, KG, KZ, RU, TJ, TM), European (AL, AT, BE, BG, CH, CY, CZ, DE, DK, (72) Inventor; and EE, ES, FI, FR, GB, GR, HR, HU, IE, IS, IT, LT, LU, LV, (71) Applicant : HENRY, David [FR/FR]; 1 Impasse des cas MC, MK, MT, NL, NO, PL, PT, RO, RS, SE, SI, SK, SM, cades, F-77210 Fontaine le Port (FR). TR), OAPI (BF, BJ, CF, CG, CI, CM, GA, GN, GQ, GW, (74) Agent: WATSON, Bruce P ; Corning Incorporated, Intel ML, MR, NE, SN, TD, TG). lectual Property Department, SP-TI-3-1, Corning, New Published: York 1483 1 (US). — with international search report (Art. 21(3)) © o (54) Title: METHOD OF DECORATING CHEMICALLY STRENGTHENED GLASS (57) Abstract: A method of decorating chemically strengthened glass. The coating deposition process entails maintaining a depos ition temperature and a curing temperature below a threshold where the chemically strengthened glass is weakened. The coating composition used in the process is a single phase and comprises alkoxysilane functionalized isocyanurate or alkoxysilane functional - ized biuret, wherein the alkoxysilane is linked to the isocyanurate or biuret by an urea linking group. METHOD OF DECORATING CHEMICALLY STRENGTHENED GLASS CROSS-REFERENCE TO RELATED APPLICATIONS [0001] This application claims the benefit of priority under 35 U.S.C § 119 of European Patent Application Serial No. 12305068.4 filed on January 19, 2012 the contents of which are relied upon and incorporated herein by reference in their entirety as if fully set forth below. BACKGROU ND [0002] The present disclosure generally relates t o a method of decorating chemically strengthened glass. [0003] There is a general desire t o decorate glass su bstrates for both aesthetic and functional purposes. Accordingly, there is a continuing drive for an efficient method of decorating chemically strengthened glass articles with a single phase coating composition. BRI EF SU MMARY [0004] According t o the present specification, a single phase coating composition for decorating chemically strengthened glass is desirable. In accordance with one embodiment of the present disclosure, a method of decorating chemically strengthened glass is provided. A chemically strengthened glass sheet is deposited with a single phase coating composition. The deposition of the coating composition on the glass sheet is done at a temperature below 400°C. The coating composition is also cured at a temperature below 400°C. The coating composition comprises at least one pigment, at least one mineral filler, and a binder comprising alkoxysilane functionalized isocyanurate or alkoxysilane functional ized biuret. The alkoxysilane is linked t o the isocyanurate or biuret by an urea linking group. [0005] In accordance with another embodiment of the present disclosure, a method of decorating chemically strengthened glass is provided. A glass sheet comprising soda lime glass, an alkali containing aluminosilicate glass, an alkali containing aluminoborosilicate glass, an alkali containing borosilicate glass, or an alkal i containing glass-ceramic is chemically strengthened by an ion-exchange process. A single phase coating composition is deposited on the glass sheet at a temperature below 300°C. The coating composition is also cured at a temperature below 300°C. The coating composition comprises at least one pigment, at least one mineral filler, and a binder comprising alkoxysilane functional ized isocyanurate or alkoxysilane functionalized biuret. The alkoxysilane is linked t o the isocyanurate or biuret by an urea linking group. The pigment is carbon black, iron pigment, cobalt pigment, cadmium pigment, chromium pigment, titanium pigment, zinc pigment, lead pigment, magnesium pigment, vanadium pigment, copper chromite black spinel, or combination thereof. The mineral filler is a silicate, alumina, zirconia, carbide, talc, clay, or combination thereof. When cured, the coating composition provides light transmittance lower than 0.2% for all wavelengths in the UV-visible wavelength range for a 25 micrometer thick cured coating and has a cross hatch adhesion score of 4 B or 5B. [0006] Additional features and advantages of the embodiments described herein will be set forth in the detailed description which follows, and in part will be readily apparent t o those skilled in the art from that description or recognized by practicing the embodiments described herein, including the detailed description which follows and the claims. [0007] It is t o be understood that both the foregoing general description and the following detailed description describe various embodiments and are intended t o provide an overview or framework for understanding the nature and character of the claimed subject matter. DETAILED DESCRI PTION [0008] Glass articles can be decorated for aesthetics or functional purposes. A conventional method of decorating glass sheets is applying ceramic enamel t o glass su bstrates using a screen printing process. The process requires high temperatures which are necessary t o fuse the ceramic enamel t o the glass substrate. The enamel typically requires a firing temperature of about 500°C t o 700°C t o fuse t o the glass substrate. Therefore, the glass must withstand these temperatures without loss of its mechanical properties and/or its shape. The high temperature requirement means decoration of thin chemically-toughened glass by means of such ceramic enamels is less desirable than low temperature methods. A major reason for the desirability of avoiding high temperatures is that the thin chemically-toughened glass rapidly loses its mechanical strength when exposed t o the high temperatures required t o fire ceramic enamel. Without wishing t o be bound by theory, the loss of mechanical strength is believed the result of thermal diffusion of ions occurring and thus degradation of the depth of layer (DOL) and compressive stress (CS) that provides the superior resistance to crack initiation and fail ure. Also high temperature processing induces distortion, such as warping, of the thin glass. [0009] Multi-phase low temperature glass decoration techniques combine two or more phases, e.g., a curing catalyst and a resin, before application to the glass and can be time consuming and limit pot life. Once the batch is mixed, it must be used within a finite time period before the coating composition cures. This is in contrast to a single phase coating composition, which is defined herein as a composition that does not require the addition of a curing catalyst prior to use. [0010] Reference will now be made in detail to embodiments of methods of making decorated chemically strengthened glass. Although the concepts of the present disclosure are presented with specific reference t o specific glass compositions, it is contemplated that the concepts will enjoy applicability to a wide variety of glass substrates where decorating is desired. [0011] According to contemplated methods of decorating chemically strengthened glass in accordance with the present disclosure, a glass sheet is provided. The glass sheet is then chemically strengthened. Further, a single phase coating composition is deposited on the glass sheet at a temperature below approximately 400°C. The coating composition comprises at least one pigment, at least one mineral filler, and a binder. The binder may comprise alkoxysilane functionalized isocyanurate or may comprise alkoxysilane functionalized biuret. The alkoxysilane is linked to the isocyanurate or biuret by an urea linking group. The deposited coating composition is then cured at a temperature below approximately 400°C. It is contemplated that the glass sheet may be chemically strengthened far in advance of the deposition step and by an entity separate and distinct from the entity undertaking the deposition step. [0012] It is contemplated that the glass sheet may be a soda lime glass, an alkali containing aluminosilicate glass, an alkali containing aluminoborosilicate glass, an alkali containing borosilicate glass, an alkali containing glass-ceramic, or other glass known by those skilled in the art. [0013] It is contemplated that the glass sheet may be chemically strengthened by an ion- exchange process or some other type of conventional or yet to be developed chemical strengthening process. The ion-exchange process may comprise exchanging Na, Li, or Na and Li ions in the surface of the glass for large alkali ions. The ion-exchange preferably occurs t o a depth of at least approximately 40 µιτι from the surface of the glass sheet.
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