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(12) Patent Application Publication (10) Pub. No.: US 2017/0037257 A1 YANG Et Al

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(12) Patent Application Publication (10) Pub. No.: US 2017/0037257 A1 YANG Et Al US 20170037257A1 (19) United States (12) Patent Application Publication (10) Pub. No.: US 2017/0037257 A1 YANG et al. (43) Pub. Date: Feb. 9, 2017 (54) GRAPHENE-BASED COATINGS Publication Classification Applicant: Board of Regents, the University of (51) Int. C. (71) C09D 5/08 (2006.01) Texas System, Austin, TX (US) C09D 7/12 (2006.01) (72) Inventors: Duck J. YANG, Flower Mound, TX C09D 5/16 (2006.01) (US); Daniel N. TRAN, Carrollton, TX (52) U.S. C. (US); Sangmin LEE, McKinney, TX CPC ............. C09D 5/084 (2013.01); C09D 5/1618 (US) (2013.01); C09D 7/1225 (2013.01); C08K 3/04 (2013.01) (21) Appl. No.: 15/304,260 (22) PCT Fed: Apr. 14, 2015 (57) ABSTRACT (86) PCT No.: PCT/US 15/25693 The present disclosure relates to coatings comprising func tionalized graphene(s) and polymers (resins). In accordance S 371 (c)(1), with the disclosure, graphene can be used with functional (2) Date: Oct. 14, 2016 ization with polymers (resins) with or without pigments, fillers, reactive catalysts or accelerators as finishes to protect Related U.S. Application Data roll steel, galvanized roll steel, equipment, automobiles, (60) Provisional application No. 61/979,341, filed on Apr. ships, construction and marine structures from corrosion, 14, 2014. fouling and UV deterioration. Patent Application Publication Feb. 9, 2017. Sheet 1 of 7 US 2017/0037257 A1 3. - 120 | R & - --- -- is is . -- --- s --& s --- ...-- s 9 :---------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------- 3 Graphene Content 3 with XXXXXXXXXXXXXXXXXXxxxxx xxxx xxxx xxxxxx xxxx xxxxx xxxx xxxx xxxx xxxx xxxx xxxx xxxxxx xxxxx xxxx xxxx xxxx xxxx xxxx xxxx xXXXXXXXXXXXXXXXXXru Adhesion Test (3.5% NaCl Solution) 13% x 1% Saak A. : R x3%. Sak x 4% Soak ---...--&S8&---------------------------- 3. Time week Patent Application Publication Feb. 9, 2017. Sheet 2 of 7 US 2017/0037257 A1 YYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYY-YYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYYY 8 8 8 8 8 8 8 8 8 8 8 8 a ri 8 : x 1% -iurid 8 ax% is 8 xxx, a His 8 8 8 8 8 8 8 8 8 8 8 8 5 : 8 8 -sess-s-s-s-s-s-s-s-s-s-s-s-s-s-s-s-s-s-s-s-s-sSSSSSSSS : 8 Patent Application Publication Feb. 9, 2017. Sheet 3 of 7 US 2017/0037257 A1 25 -----------------------------------------Š ..................................S.................. Graphene Content vs Contact Angle Artistic GioSS Warnish Patent Application Publication Feb. 9, 2017. Sheet 4 of 7 US 2017/0037257 A1 Graphene Content vs Contact Angle Dammar Warnish 85 8 7 5. 9. 2% Graphene Content (% wt) FIG. 7 Graphene Content vs Contact Angle Acrylic Warnish a :--------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------------- Og 98. 2% Graphene Content (% wt) Patent Application Publication Feb. 9, 2017. Sheet 5 of 7 US 2017/0037257 A1 Goss 0% graphere sex 2% graphere 78 graphere 2O 250 38 350 40 wavelength (nm) FIG. 9 ana: Wanist % graphene as 4% galee 28 25 33 35 a. wavefuniper {fi} FIG 10 Patent Application Publication Feb. 9, 2017. Sheet 6 of 7 US 2017/0037257 A1 Acrylic Goss O% graphene rew 2% graphene - 4% graphene 2 25 3. 35 4. wavelength (nm) FIG 11 Base coat Concrete Base Stetref : stal Sustrates FIG. 12 Tap coat ŠaBassŠ at Prie? wer Metal Slustrate Iron Steel fetc. FIG 3 Patent Application Publication Feb. 9, 2017. Sheet 7 of 7 US 2017/0037257 A1 Topcoat rass coat Prier Syro-Escaat line phosphate S SS: &S :r8 Zinc FIG. 14 US 2017/0037257 A1 Feb. 9, 2017 GRAPHENE-BASED COATINGS wherein the composition is used as a coating. In some embodiments, the binder is a polymeric binder. In some 0001. The present application is a national phase appli embodiments, the binder is an urethane resin, an epoxy cation under 35 U.S.C. S371 of International Application resin, acrylic resin, or an alkyd resin. In some embodiments, No. PCT/US2015/025693, filed Apr. 14, 2015, which claims the binder comprises two or more components. The binder benefit of priority to U.S. Provisional Application Ser. No. may also further comprise two components wherein at least 61/979,341, filed Apr. 14, 2014, the entire contents of each one of the components is a resin further comprising a of which are hereby incorporated by reference. catalyst. In some embodiments, the resin further comprising BACKGROUND a catalyst is DPX 1 with DPX 2. The binder may be DPX-170, DPX-171, DPX-172, or DPX-173. 0002 A. Field 0013. In some embodiments, the functionalized graphene 0003. The present disclosure relates to coatings compris is present in a layer consisting of a depth of 1 to 10 sheets ing graphene and polymers (resins) and potentially fillers of functionalized graphene. In some embodiments, the depth and pigments. In accordance with the description, graphene of the functionalized graphene consists of 1, 2, 3, or 4 sheets can be used with functionalization with polymers (resins) through more than 50% of the coating. The coating may including reactive catalysts or accelerators as finishes to comprise from about 0.5-20 wt % of functionalized gra protect roll steel, galvanized roll Steel, automobiles, equip phene. In some embodiments, the coating comprises 0.5-10 ment, ships, construction and marine structures from corro wt % of functionalized graphene. The coating may comprise sion, fouling and UV deterioration. 1-5 wt % of functionalized graphene. In some embodiments, 0004 B. Background the coating comprises 0.5,0.75, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 0005. The technology encompasses the combination of 12.5, or 15 wt %, or any range derivable thereof. In some graphene with polymers to perform as corrosion and fouling embodiments, the coating comprises functionalized gra resistant and UV absorbing and hydrophobic finishes for roll phene present in a layer from about 0.001 to 10 um. The steel, galvanized roll steel, automobiles, ships, construction layer may be from about 0.01 to 5 um or from about 0.05 to and marine structures. The multi-functional properties of 2 Lum. graphene Such as hydrophobicity. It to It stacking (self 0014. In some embodiments, the functionalized graphene assembly), UV absorption and barrier with a high surface comprises one or more functional groups selected from: area (2,630 sqm/gram) provide the finishes with anti-cor amino, cyano, hydroxyl, carboxylic acid, isocyanate, alde rosion, anti-fouling, hydrophobic and UV absorbing func hyde, epoxide, urea, or anhydride. tions in finishes. 0015. In some embodiments, the compositions further 0006 Surface coatings can used to impart articles with comprise a carrier. The carrier may be water or an organic desirable properties that are not possessed by the articles Solvent selected from an aliphatic compound; an aromatic themselves or not possessed in a sufficient degree. Many of compound; mineral spirits; methyl ethyl ketone; n-butyl these drawbacks can be overcome by the use of polymeric acetate; ethanol, isopropanol, t-butyl alcohol; and ethylene materials, which can have cost, weight, processability, and glycol, and mixtures thereof. In some embodiments, the flexibility of design advantages over metals. However, most aliphatic compound is hexanes. In other embodiments, the polymer materials are not intrinsically electrically or ther aromatic compound is toluene or Xylene. The compositions mally conductive enough for many applications. Conductive may further comprise a filler. In some embodiments, the polymeric resin compositions can be made in Some cases by filler is treated clays, calcium carbonate powders, alumino adding fillers to polymers, but high loadings are often silicate fine powders, fine-particle-size silica aerogel-type required, which can be to the detriment of physical and other pigments, and ultrahigh-molecular-weight polymers such as properties of the materials, as well as lead to melt processing modified cellulosic polymers, natural polymers like carra difficulties when thermoset materials are used, among other geenan, and high-molecular-weight water-soluble polymers. possible drawbacks. The composition may further comprise a pigment. In some 0007 Coatings can also be used for countless other embodiments, the pigment is a fine particle ranging in size applications, including providing moisture resistance, cor from 0.01 to 100 um like carbon black, TiO, Zinc oxide, rosion resistance, UV radiation resistance, abrasion resis antimony oxide, iron oxide (inorganic) Zinc powder, alumi tance, thermal conductivity, impact resistance, stiffness, and num metal flake, or an organic dye selected from the dye many others. classes of diazo, phthalocyanine, or quinacridone com 0008. It would be desirable to obtain coatings that can be pounds, or another pigment known in the art. The compo used with a wide variety of substrates to provide useful sitions may further comprise a dispersant. In some embodi properties. ments, the dispersant is alkali polyphosphate, alkali poly acrylate, poly-ethylene glycol, linear alkylbenzene SUMMARY Sulfonate, or other dispersants know in the art 0009 Disclosed and claimed herein is coatings compris 0016. In yet another aspect, the present disclosure pro ing graphene and polymers (resins) and which may further vides methods of coating a Substrate comprising: applying a comprise fillers and pigments. Further disclosed and claimed composition described herein to the surface of the substrate herein is a method for coating a Substrate with a coating to form a coating on the surface of the substrate. The comprising graphene and polymers (resins) and fillers and Substrate may be made of metal or may be made of a pigments. polymer. The substrate may be made of fabric, textile, or 0010. In one aspect, the present disclosure provides com pulp. positions comprising: 0017. In some embodiments, the coating is from about 0011 (A) functionalized graphene; and 0.1 um to about 10 mm (millimeters) thick. The coating may 0012 (B) a binder, be from about 0.1 um to about 300 um thick.
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