PPPoster Session, Thursday, June 17Theme F686 - N1123The Effect of Nanometer Size Mica Fillers on Mechanical Properties of Polyurethane112UAysel Ersoy YilmazUP P*, Ayten KuntmanP Pand Bulent AydemirP1PDepartment of Electrical-Electronics Eng, Istanbul University, Istanbul 34380, Turkey2PTubitak UME, National Metrology Institute, Gebze, Kocaeli 41470, TurkeyAbstract-In this study mechanical properties of nanometer size mica added polyurethanes were <strong>in</strong>vestigated experimentally. At first micaparticles at 1 nanometer size were prepared, and then polyurethane samples with different nanometer size mica concentrations were prepared.Except 10 % mica filler concentrations the result<strong>in</strong>g nano composites compressive strength is <strong>in</strong>creased.Today <strong>in</strong> many eng<strong>in</strong>eer<strong>in</strong>g applications, more than oneclass of materials is used together. At this po<strong>in</strong>t additives andfillers ga<strong>in</strong> extra importance due to their significant impact onelectrical, thermal, mechanical and environmental propertiesof the result<strong>in</strong>g composite. Polyurethanes have a wide rage ofapplications <strong>in</strong>clud<strong>in</strong>g coat<strong>in</strong>gs, adhesives, fibers, thermal<strong>in</strong>sulator, electrical <strong>in</strong>sulators, etc. However they have somedisadvantages such as low mechanical strength, low thermalstability, low electrical properties, etc. Dur<strong>in</strong>g the last decadeseveral studies has been done to improve these propertiesus<strong>in</strong>g nano size particles [1-5].In this study polyurethane nano composite with various micaconcentrations is studied. To <strong>in</strong>vestigate the change <strong>in</strong>mechanical properties compressive strength tests were doneaccord<strong>in</strong>g to the ASTM D1621-04a standard.In this study micas were modified with am<strong>in</strong>olauric acid andthe preparation procedure was briefly given. Biotite(KMg2.5Fe2+0.5AlSi3O10(OH)1.75F0.25 ) which has adensity of 2,9 g/cm3 is used as mica filler. To a suspension ofam<strong>in</strong>olauric acid (8.61 g, 40 mmol) <strong>in</strong> 1,000 ml distilledwater, concentrated HCl (4.17 g, 40 mmol) was added. Themixture was stirred at 80 C until gett<strong>in</strong>g a clear solution<strong>in</strong>dicat<strong>in</strong>g the formation of ammonium salt. To this solution, asuspension of 20 g of mica <strong>in</strong> 1,000 ml of distilled water wasadded with mechanical stirr<strong>in</strong>g at 80 C. The stirr<strong>in</strong>g wascont<strong>in</strong>ued over night. The resulted white precipitate wascollected by suction filtration. The precipitate was suspended<strong>in</strong> hot distilled water with mechanical stirr<strong>in</strong>g for 1 h toremove the adsorbed salts. This process was repeated severaltimes until no chloride ions were detected <strong>in</strong> the filtrate whenadd<strong>in</strong>g 0.1 M AgNO3. The precipitate was dried <strong>in</strong> a ventedoven at 60 oC for 3 days and then at 80 oC under 0.01 atm.vacuum for 24 h.All the polyurethane nano composite samples were preparedunder the same laboratory conditions. The desired weights ofpolyurethane, mica and %0.01 Di butylt<strong>in</strong> dilaurate catalystwas mixed for 5 m<strong>in</strong>utes. Then the mixture was heated to 100oC and 25% polymeric (methylenediphenylene diisocyanate)MDI was added. The new blend was poured <strong>in</strong>to the mouldand pressed for 10 m<strong>in</strong>utes with the help of clamps. Mouldwas placed <strong>in</strong> a degasser under high vacuum to remove any airand potentially water vapor from the system. 24 h later themould was opened and the samples were cut <strong>in</strong> the dimensionsof 1mm by 50mm by 50mm. The highest content of mica <strong>in</strong>polyurethane samples was limited to 10 % by weight for nanofillers due to dispersion and process<strong>in</strong>g problems.The mechanical tests to determ<strong>in</strong>e compressive strength werecarried out on samples prepared accord<strong>in</strong>g to the ASTMD1621-04a standard. The experiments were carried out with aZwick tensile test mach<strong>in</strong>e at National Metrology Institute <strong>in</strong>TUBITAK. For the compressive strength tests, the sampleswere shaped <strong>in</strong>to 12.3 mm diameter, 25.4 mm long cyl<strong>in</strong>ders.The test parameters can be adjusted with TestXpert software.Tests were performed at a speed of 1.00 mm/m<strong>in</strong>. All testswere performed at 23 C (room temperature).Table 1. Compressive strength test results for 1 nm particle sizeMaterial Type Compressive Strength (GPa)Pure PU 9,056PU+%1 11,426PU+%3 11,600PU+%5 9,541PU+%10 7,816The preparation of PU nanocomposite foams were described<strong>in</strong> this study. Clay dispersion is affect by chemical process.With the <strong>in</strong>clusion of 3% micas, nanocomposite show asmaller cell size than pure polyurethane samples. Depend<strong>in</strong>gon the chemical structure of polyurethane, as high as 28%<strong>in</strong>crease <strong>in</strong> compressive strength were observed <strong>in</strong> PU-micananocomposite. However <strong>in</strong>creas<strong>in</strong>g the filler content to 10%mica concentration opposite effect was observed <strong>in</strong> PUnanocomposite 13.6% decrease <strong>in</strong> compressive strength wereobserved. Preparation of polyurethane nanocomposite is acomplicated process where many factors could effect bubblenucleation and bubble growth and <strong>in</strong> turn the compressivestrength. For applications <strong>in</strong> electrical <strong>in</strong>sulators, compressivestrength is a very important property to calculate the mass ofcover material upon the bare cable conductor. Accord<strong>in</strong>g tothe results from this study cell size <strong>in</strong> polyurethane nanocomposite is decreased and compressive strength isremarkably <strong>in</strong>creased at 3% mica addition. However detailedmechanism on how nano size mica particles affect mechanicalproperties of polyurethanes needs further <strong>in</strong>vestigation.*Correspond<strong>in</strong>g author: aersoy@istanbul.edu.tr[1] R. A. C. Altafim, C. R. Murakami, S. C. Neto, L. C. R. Araújo,G. O. Chierice, “The Effects of Fillers on Polyurethane Res<strong>in</strong>-basedElectrical Insulators”, Materials Research, Vol 6, No 2, pp. 187-191,2003.[2] X. Cao, L. J. Lee, T. Widya, C. Macosko, “Polyurethane/claynanocomposites foams: process<strong>in</strong>g, structure and properties”,Polymer , Vol. 46, pp.775-783, 2005.[3] J.H. Chang, Y. U. An, “Nanocomposites of Polyurethane withVarious Organoclays: Thermomechanical Properties, Morphology,and Gas Permeability”, Journal of Polymer Science: Part B: PolymerPhysics, Vol. 40, pp. 670–677, 2002 .[4] F. Sa<strong>in</strong>t-Michel, L. Chazeau, J.-Y. Cavaille, “Mechanicalproperties of high density polyurethane foams: II Effect of the fillersize”, Composites Science and Technology Vol. 66, pp. 2709–2718,2006. .[5] K.J. Yao, M. Song, D.J. Hourston, D.Z. Luo, “Polymer/layeredclay nanocomposites: 2 polyurethane nanocomposites”, PolymerCommunication, Vol. 43, pp.1017-1020, 2002.6th Nanoscience and Nanotechnology Conference, zmir, 2010 729
Poster Session, Thursday, June 17Theme F686 - N1123MWCNT-Al 2 O 3 Hybrids Dispersed <strong>in</strong> Epoxy CompositesSeda Aksel 1 , Özge Malay 1 , Dom<strong>in</strong>ik Eder 2 , Yusuf Z. Menceloğlu 1, *1 Sabanci University, Materials Science and Eng<strong>in</strong>eer<strong>in</strong>g Program, İstanbul,34956, Turke.2 University of Cambridge, Department of Materials Science and Metallurgy, Cambridge, UKAbstract— This work aims to <strong>in</strong>vestigate dispersion state and thermo-mechanical properties of alum<strong>in</strong>ium oxide (Al 2 O 3 ) coated multi- walledcabon nanotubes (MWCNTs) <strong>in</strong> epoxy matrix. MWCNT-<strong>in</strong>organic hybrids were <strong>in</strong>troduced as an efficient filler to reduce entangledagglomerates <strong>in</strong> epoxy res<strong>in</strong> with improved thermal and mechanical characteristics.Carbon nanotube (CNT)-<strong>in</strong>organic hybrids are a new class ofmaterials that carbon nanotubes are coaxially coated with<strong>in</strong>organic components. These materials show superior optical,mechanical, electrical and thermal properties with respect to thephysical nature of <strong>in</strong>organic component [1].Previous studies which focus on addition of <strong>in</strong>organicnanoparticles <strong>in</strong>to carbon nanotube/epoxy nanocomposite alsoproved that <strong>in</strong>organic nanoparticles dim<strong>in</strong>ish the agglomerationof carbon nanotubes <strong>in</strong> polymeric matrix [2]. This workprimarily concentrates on coat<strong>in</strong>g of carbon nanotubes withalum<strong>in</strong>ium oxide (Al 2 O 3 ) <strong>in</strong> order to improve dispersion ofcarbon nanotubes <strong>in</strong> epoxy matrix and to characterize CNT-Al 2 O 3 /epoxy nanocomposites prior to its use for specificapplications with respect to enhanced thermal, mechanical andelectrical properties.Multi-walled carbon nanotubes (MWCNTs) which wereprepared by chemical vapor deposition (CVD) method, wereused <strong>in</strong> this study. The average diameter of the nanotubes is 70nm and the length range is 100-200 μm. MWCNTs were coatedwith <strong>in</strong>organic components via sol-gel process. Benzyl alcoholwas used to functionalize hydrophobic surface of MWCNTs viathe π-π <strong>in</strong>teraction between the aromatic MWCNT surface andbenzyl r<strong>in</strong>g of benzyl alcohol [1,3].MWCNTs, benzyl alcohol functionalized MWCNTs andAl 2 O 3 –MWCNT hybrids were used as filler and eachnanocomposite film conta<strong>in</strong>s 0.05 wt% filler. The polymermatrix used for the composites was an epoxy based system witham<strong>in</strong>e hardener.Solid State13 C-NMR spectroscopy of functionalizedMWCNTs clearly shows the presence of -CH 2 group bonded tohydroxyl group (-OH) on the surface of MWCNTs by the peakat 62 ppm. Al 2 O 3 coat<strong>in</strong>g on MWCNTs hybrid was confirmed byXRD and SEM/EDX analyses as shown <strong>in</strong> Figure 1 (a,b). Inaddition to graphite peaks at 2θ values of 26 and 44 <strong>in</strong> the XRDplot of MWCNTs, alum<strong>in</strong>a peak was observed at 39 for Al 2 O 3 -MWCNT hybrid. Weight percentage of alum<strong>in</strong>ium and oxygen<strong>in</strong> the sample detected by EDX analysis also confirmed thatsample was derived from the Al 2 O 3 molecules <strong>in</strong> Figure 2 (a,b).Optical microscope images <strong>in</strong> Figure 3 (a,b,c,d), which showdispersion state of MWCNTs <strong>in</strong> uncured epoxy res<strong>in</strong>, demostratethat degree of filler dispersion <strong>in</strong>creases along with functionalizedMWCNTs and hybrids.Figure 3. MWCNT dispersion <strong>in</strong> uncured epoxy matrix (a) 0.05 wt%MWCNTs (b) 0.05 wt% functionalized MWCNTs (c) 0.05 wt%MWCNT-Al 2 O 3 hybrids (d) 0.05 wt% MWCNT, 0.2 wt% Al 2 O 3 hybrids.MWCNT-Al 2 O 3 hybrids could be homogeneously dispersed <strong>in</strong>epoxy res<strong>in</strong> due to the less attractive forces between carbonnanotubes. SEM (Scann<strong>in</strong>g Electron Microscopy) images <strong>in</strong>Figure 4 (a,b,c) show that functionalization of MWCNTs anduniform coat<strong>in</strong>g by Al 2 O 3 decrease the degree of agglomeration.S<strong>in</strong>ce the free surface area of carbon nanotubes reduces, weakelectrostatic forces provided via <strong>in</strong>organic coat<strong>in</strong>g decreases theentanglement degree.(a) (b) (c)Figure 4. SEM image of (a) MWCNTs (b) BA-functionalized MWCNTs(c) MWCNT-Al 2 O 3 hybrids.Addition of MWCNTs decreases the glass transition temperature(Tg) due to lower cross-l<strong>in</strong>k<strong>in</strong>g degree of the epoxy matrix.Addition of benzyl alcohol and coat<strong>in</strong>g MWCNTs by Al 2 O 3reduces the decrease of Tg with respect to <strong>in</strong>crease <strong>in</strong> dispersionstate of the filler. On the other hand, 3-po<strong>in</strong>t bend<strong>in</strong>g analysisreveals that both flexural strength and flexural modulus of thenanocomposites <strong>in</strong>creases via functionalization of the MWCNTs.In summary, MWCNTs were uniformly coated with an <strong>in</strong>organiccomponent, Al 2 O 3 . New filler type was developed to atta<strong>in</strong> novelAl 2 O 3 -MWCNT/epoxy nanocomposite materials.*Correspond<strong>in</strong>g author: yusufm@sabanciuniv.eduFigure 1.a. XRD Plotof the MWCNTsFigure 1.b. XRD Plot of theAl 2 O 3 -MWCNT HybridsFigure 2.a. EDX Spectrum Figure 2.b. EDX Spectrum ofof the MWCNTs the Al 2 O 3 -MWCNT Hybrids[1] Eder, D., W<strong>in</strong>dle, A. H., 2008. Carbon-Inorganic Hybrid Materials:The Carbon-Nanotube/TiO 2 Interface, Advance Materials 20: 1787-1793.[2] Sumfleth, J., Prado, L.A, Sriyai, M., Schulte, 2008. K., Titania-dopedmulti-walled carbon nanotubes epoxy composites: Enhanceddispersion and synergistic effects <strong>in</strong> multiphase nanocomposites, Polymer49: 5105-5112.[3] Eder, D., W<strong>in</strong>dle, A. H., 2008. Morphology control of CNT-TiO 2hybrid materials and rutile nanotubes, Journal of Materials Chemistry18: 2036-2043.6th Nanoscience and Nanotechnology Conference, zmir, 2010 730
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