Poster Session, Thursday, June 17Theme F686 - N1123UV CURABLE B/F/Si CONTAINING HYBRID MATERIALSBihter Zeytuncu, 1* M.Vezir Kahraman 2 and Onuralp Yucel 11 Applied Research Center of Materials Science and Production Technology, Istanbul Technical University, Istanbul 34469, Turkey2 Department of Chemistry, Marmara University, Istanbul 34722, TurkeyAbstract — A series of UV-curable boron/flour/silicon conta<strong>in</strong><strong>in</strong>g hybrid coat<strong>in</strong>gs prepared by anhydrous sol-gel technique.The chemical structure of hybrid coat<strong>in</strong>gs was characterized by FT-IR, RT-IR, 1 H-NMR and 29 Si-CP MAS-NMR techniques.UV curable coat<strong>in</strong>gs were applied on polycarbonate substrates. The physical and mechanical properties of UV-cured coat<strong>in</strong>gssuch as pendulum hardness, pencil hardness, contact angle, gel content, MEK rubb<strong>in</strong>g test, tensile test, abrasion resistance,chemical resistance, flame retardant, anti-sta<strong>in</strong> and gloss were exam<strong>in</strong>ed. Thermal gravimetric analysis (TGA) was made.Results of all analysis conducted on free films and coat<strong>in</strong>gs were discussed. The morphology of the hybrid materials wasexam<strong>in</strong>ed by SEM. The hybrids were nanocomposites.Sol-gel is widely used method for the preparation oforganic-<strong>in</strong>organic hybrid based coat<strong>in</strong>g materials [1].Organic-<strong>in</strong>organic hybrid materials comb<strong>in</strong>e theadvantages of either elasticity, impact resistance of organicpolymers and the high mechanical strength, chemicalresistance, thermal stability, optical qualities of the<strong>in</strong>organic materials. The UV curable hybrid coat<strong>in</strong>gsprepared by sol-gel method, have low cost, fast cur<strong>in</strong>g, lowviscosity and long time duration [2,3]. The UV curablehybrid coat<strong>in</strong>g materials have good adhesive, hardness,good mechanical and chemical properties, which aresensitive to the environment [4].The aim of this study was to prepare and characterizeUV-curable, boron/flour/silicon-conta<strong>in</strong><strong>in</strong>g epoxy acrylatebased organic-<strong>in</strong>organic hybrid coat<strong>in</strong>gs hav<strong>in</strong>g abrasionand flame resistant, anti-sta<strong>in</strong> and high gloss properties.Therefore, <strong>in</strong> the first stage; borate ester was synthesized.Then, hybrid coat<strong>in</strong>gs hav<strong>in</strong>g various concentrations ofboron/flour/silicon were prepared and applied on toPolycarbonate panels and were hardened by UVirradiation. The prepared hybrid coat<strong>in</strong>gs werecharacterized by the analysis of various properties such ashardness, abrasion and chemical resistance, flameretardancy, gloss and stress–stra<strong>in</strong> tests. The thermal andmorphological behavior of the hybrid coat<strong>in</strong>gs was alsoevaluated.The solvent resistance of coat<strong>in</strong>gs was exam<strong>in</strong>ed byperform<strong>in</strong>g the MEK rubb<strong>in</strong>g test. The solvent resistanceis excellent; exceed<strong>in</strong>g 500 MEK double rubs while pencilhardness is greater than 5H, also <strong>in</strong>dicative of highly crossl<strong>in</strong>kedfilm. The gel content of polymeric films was foundto be between 98 to 99,7 %. The cross-cut adhesionexperiment showed that 100 % adhesion was reached forall coat<strong>in</strong>gs. The chemical resistance of all hybrid coat<strong>in</strong>gswas also <strong>in</strong>vestigated by immers<strong>in</strong>g samples <strong>in</strong> variousreagents (10 % NaOH, 10 % HCl, 10 % H 2 SO 4 , Xylene)for 24 h time period. The general physical appearance ofsamples was perfect and no cracks were observed.Abrasion resistance is often characterized by the Taberabrasermethod measur<strong>in</strong>g the mass decrease caused by themechanical degradation of protective layers that is treatedby abrad<strong>in</strong>g gr<strong>in</strong>ders. The high boron/flour/silicon contentdemonstrated a better protective performance <strong>in</strong>comparison to other formulations. The LOI values of thesecoat<strong>in</strong>gs <strong>in</strong>creased from 20.4 to 23.1. The thermaloxidative stability of the hybrid coat<strong>in</strong>g was <strong>in</strong>vestigatedby thermo gravimetric analysis (TGA) technique <strong>in</strong> airatmosphere. The maximum weight loss temperature wasraised to 425 ◦C. The enhancement of <strong>in</strong>corporation ofB/F/Si on the thermal stability of epoxyacrylate res<strong>in</strong>s wasthus demonstrated. Therefore it is concluded that thethermal stability of epoxy acrylate res<strong>in</strong> is enhanced byadd<strong>in</strong>g B/F/Si as a flame retardant. The morphology of thefractured surfaces was observed by scann<strong>in</strong>g electronmicroscopy (SEM). Figure 1 presents the SEM image ofthe hybrid coat<strong>in</strong>g material. The SEM micrograph showspherical borosilicate particles are distributed with<strong>in</strong> thehybrid system. The approximate particle size is less than100 nm.Figure 1: SEM micrograph of the hybrid coat<strong>in</strong>gIn summary, UV curable boron conta<strong>in</strong><strong>in</strong>g organic<strong>in</strong>organichybrid coat<strong>in</strong>g was prepared by anhydrous solgeltechnique. The properties of boron-conta<strong>in</strong><strong>in</strong>g hybridcoat<strong>in</strong>g materials such as hardness, chemical and abrasionresistance were improved. All hybrid coat<strong>in</strong>gs wereobta<strong>in</strong>ed crack free and transparent. The solvent andchemical resistance experiments proved that all the hybridmaterials are promis<strong>in</strong>g as a candidate for the relatedapplications. On the other hand thermal and flameretardantproperties of hybrid coat<strong>in</strong>gs were improved bythe <strong>in</strong>creas<strong>in</strong>g of B/F/Si content. The morphology studies<strong>in</strong>dicate that, the nanometer-scaled <strong>in</strong>organic particlesdisperse homogenously <strong>in</strong> the hybrid system.*Correspond<strong>in</strong>g author: bihter_zeytuncu@hotmail.com[1] Br<strong>in</strong>ker, C.J.; Scherer, G.W.: "Sol-Gel Science: The Physicsand Chemistry of Sol-Gel Process<strong>in</strong>g"; Academic Press, NewYork, USA, (1990).[2] Holman, R.; Oldr<strong>in</strong>g, P.; “UV& EB cur<strong>in</strong>g formulation forpr<strong>in</strong>t<strong>in</strong>g <strong>in</strong>ks, coat<strong>in</strong>gs and pa<strong>in</strong>t<strong>in</strong>gs”, London (1998).[3] Odian, G.: "Pr<strong>in</strong>ciples of Polymerization"; Fourth Edition;Wiley Interscience, New York, USA, (2004) 96.[4] Cho, J:; Kim, E.; Kim, H.K.; Hong, J.: “An <strong>in</strong>vestigation ofthe surface properties and cur<strong>in</strong>g behaviour of photocurablecationic films photosensitized by anthracene” Polymer Test<strong>in</strong>g,21 (2002) 781.[5] Kahraman, M.V., Boztoprak,Y., Güngör, A., Apohan, A.K.,Progress <strong>in</strong> Organic Coat<strong>in</strong>gs 66 (2009) 52–58.6th Nanoscience and Nanotechnology Conference, zmir, 2010 707
Poster Session, Thursday, June 17Theme F686 - N1123The Maleimide Modified Epoxy Res<strong>in</strong>s for the Preparation of UV-Curable Hybrid Coat<strong>in</strong>gsZerr<strong>in</strong> Altınta *, Sevim Karata¸ Nilhan Kayaman-Apohan and Atilla GüngörMarmara University, Department of Chemistry 34722 Istanbul/TurkeyAbstract: In the present study, maleimide-modified epoxide res<strong>in</strong> conta<strong>in</strong><strong>in</strong>g UV-curable hybrid coat<strong>in</strong>g materials were prepared and coatedon polycarbonate substrates <strong>in</strong> order to improve their surface properties. The coat<strong>in</strong>g formulations with different compositions were preparedfrom UV-curable bismaleimide-based epoxy oligomer and sol–gel mixture. The thermal and morphological properties of these coat<strong>in</strong>gsmaterials were <strong>in</strong>vestigated by us<strong>in</strong>g TGA and SEM techniques. The thermal characteristics of UV curable hybrid films were found to bebetter than without Bismaleimide and sol-gel precursor.Polymers of N-substituted maleimides and theirderivatives hav<strong>in</strong>g a rigid imide r<strong>in</strong>g <strong>in</strong> the backbone areknown as high performance polymers. Among them,bismaleimides (BMIs) have attracted much attentionbecause of their high-temperature resistance, high glasstransitiontemperature, excellent chemical and corrosionresistance, and low cost. Bismaleimide res<strong>in</strong>s are anaddition-type polyimide class of macromolecularcompounds produced from bismaleimide monomers andconta<strong>in</strong> unsaturated end groups. Bismaleimides cappedprepolymers are cured <strong>in</strong>to a highly cross-l<strong>in</strong>ked networkby additional reactions without the evolution of volatileby-products. However, due to their high cross-l<strong>in</strong>k density,they are often brittle, result<strong>in</strong>g <strong>in</strong> low impact and fracturetoughness. Introduction of a long, flexible epoxy cha<strong>in</strong> <strong>in</strong>tothe backbone of bismaleimides is expected to reduce crossl<strong>in</strong>kdensity and also to improve fracture toughness bydissipat<strong>in</strong>g the impact energy along the entire molecularcha<strong>in</strong> [1].Currently, to meet the demand of highly m<strong>in</strong>iaturizedelectronic devices, non-l<strong>in</strong>ear optical applications, and thedevelopment of next generation spacecrafts, furtherimprovement <strong>in</strong> the high performance polymers is needed.Organic–<strong>in</strong>organic hybrid coat<strong>in</strong>gs offer the opportunity tocomb<strong>in</strong>e the desirable properties of organic polymers(elasticity, processability) and <strong>in</strong>organic solids (hardness,chemical <strong>in</strong>ertness, and thermal resistance). Close to theexcellent properties of the obta<strong>in</strong>ed coat<strong>in</strong>gs,photopolymerization process itself affords advantages suchas very high reaction rates at room temperature and spatialcontrol of polymerization. These materials manifest someadvantages such as low optical propagation loss, highchemical, and mechanical stabilities as well as goodcompatibility with different surfaces to be coated [2-3].Hence, <strong>in</strong> this work, a novel bismaleimide wassynthesized by the reaction of cycloaliphatic diepoxidewith N-(carboxyphenyl) maleimide. Afterwards, thehybrid coat<strong>in</strong>gs based on UV-curable bismaleimide cappedcycloaliphatic epoxy oligomer were prepared by sol–gelmethod to <strong>in</strong>vestigate the coat<strong>in</strong>g properties. The hybridmaterials were characterized by analysis of hardness,gloss, adhesion, and stress–stra<strong>in</strong>. The thermal andmorphological behaviors of the coat<strong>in</strong>g were alsoevaluated.Table 1. TGA analysis of coat<strong>in</strong>g networksSamples60CF25CF-35BMI25CF-35BMI-5Si25CF-35BMI-10Si25CF-35BMI-15SiFirstweightloss( O C)355360355360355Max.weightloss( O C)445445445445445F<strong>in</strong>alweightloss( O C)595625630635645In conclusion, a series of UV-curable organic-<strong>in</strong>organichybrid coat<strong>in</strong>gs were prepared based on sol–gel reactionsfor TEOS and MAPTMS <strong>in</strong> the presence of epoxymodified Bismaleimide oligomer (BMI) and urethaneacrylate oligomer (UA). Incorporation of bismaleimidemodified epoxy res<strong>in</strong> <strong>in</strong>to the organic part strongly<strong>in</strong>creased the thermal resistance of hybrid samples. Upon<strong>in</strong>creas<strong>in</strong>g the <strong>in</strong>organic content of the coat<strong>in</strong>g material,thermal, mechanical, and other properties, such ashardness, gloss, contact angle, and abrasion resistance,were also improved. Corona-treated polycarbonate testpanels facilitated the adhesion of the coat<strong>in</strong>g materials. Allhybrid coat<strong>in</strong>gs were obta<strong>in</strong>ed crack-free and transparent.Furthermore, the <strong>in</strong>crease <strong>in</strong> the contact angle data of thehybrid coat<strong>in</strong>gs demonstrated the formation ofhydrophobic surface.*Correspond<strong>in</strong>g author: alt<strong>in</strong>tas_zerr<strong>in</strong>@hotmail.com[1] F. Yılmaz, L. Cianga, Y. Gu¨ ner, L. Toppare, Y. Yacı,Polymer, 45, 5765, (2004).[2] H. Tang, W. Li, X. Fan, X. Chen, Z. shen, O. Zhou, Polymer,50,1414 (2009).[3] L. A. White, J. W. Weber, L. J. Mathias, Polym. Bullet<strong>in</strong> , 46,339, (2001).6th Nanoscience and Nanotechnology Conference, zmir, 2010 708
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