Poster Session, Thursday, June 17Theme F686 - N1123Synthesis and Characterization of Polyimide-silver Nanocomposite Conta<strong>in</strong><strong>in</strong>g Chalcone Moieties <strong>in</strong>The Ma<strong>in</strong> Cha<strong>in</strong> by UV-radiationKhalil Faghihi 1 *, Meisam Shabanian 11 Organic Polymer Research Laboratory, Department of Chemistry, Faculty of Science, Arak University, Arak, 38156, Iran,Abstract-The soluble polyimide (PI)-silver nanocomposite (PISN) 6a conta<strong>in</strong><strong>in</strong>g chalcone moieties as a photosensitive group was synthesizedsuccessfully by a convenient ultraviolet irradiation technique. A precursor such as AgNO 3 was used as the source of the silver particles.Polyimide 6 as a source of polymer was synthesized by the one-step synthesis of polyimide from polycondensation reaction of 4,4'-diam<strong>in</strong>ochalcone 4 with pyromellitic anhydride 5 <strong>in</strong> the presence of iso-qu<strong>in</strong>ol<strong>in</strong>e solution. The result<strong>in</strong>g composite film was characterized by FTIRspectoscopy, X-ray diffraction (XRD), scann<strong>in</strong>g electron microscopy (SEM), thermogravimetry (TGA) and diffrantial scann<strong>in</strong>g calorimetry(DSC).There is <strong>in</strong>tense <strong>in</strong>terest <strong>in</strong> the synthesis and properties ofmetal clusters and nanoparticles prepared <strong>in</strong> both aqueous andorganic solutions and prepared <strong>in</strong> condensed state, for<strong>in</strong>stance, polymers, zeolites and glasses. Clusters,nanoparticles and its conta<strong>in</strong><strong>in</strong>g materials are potentiallyuseful <strong>in</strong> a wide range of application, <strong>in</strong>clud<strong>in</strong>g highly activecatalysts [1], magnetic materials, quantum dots andm<strong>in</strong>iaturization of electronic devices and nonl<strong>in</strong>ear opticalmaterials [2-5]. In this work, we <strong>in</strong>vestigated the preparationof new polyimide (PI)-silver nanocomposite by convenientultraviolet irradiation technique at room temperature. Thesilver nanoparticles were homogeneously dispersed <strong>in</strong> the PImatrix and the PI–silver nanocomposites exhibited anultraviolet–visible (UV-vis) absorption peak, correspond<strong>in</strong>g tothe characteristic surface plasmon resonance of silverparticles.Polyimide 6 as a source of polymer was synthesized by theone-step synthesis of polyimide from polycondensationreaction of 4,4'-diam<strong>in</strong>o chalcone 4 with pyromelliticanhydride 5 <strong>in</strong> m-cresol solution and <strong>in</strong> the presence of isoqu<strong>in</strong>ol<strong>in</strong>eas a base (Figure 1).Figure 2. SEM image of polyimide-silver nanocomposite 6aIn summery <strong>in</strong> this work, a polyimide-silver nanocompositeconta<strong>in</strong><strong>in</strong>g chalcone moieties was successfully prepared by aconvenient reduction of silver by ultraviolet irradiationtechnique. From the SEM and XRD <strong>in</strong>vestigations, the silvernanopaticles homogeneously dispersed <strong>in</strong> the PI matrix. In theUV–vis absorption spectra of the PI-silver nanocomposite, theabsorption peak due to the surface plasmon resonance of silverparticles was observed at 418 nm. Because of the goodthermal properties and Due to presence chalcone moieties <strong>in</strong>polymer backbone, these silver/PI nanocomposites can bephotosensitive and has the potential for use <strong>in</strong>microfabrication of conductive components <strong>in</strong> microelectronic<strong>in</strong>dustry.*Correspond<strong>in</strong>g author: k-faghihi@araku.ac.irFigure 1. Synthetic route of PI 6The soluble PI–silver nanocomposite was prepared by us<strong>in</strong>gultraviolet irradiation is presented. A precursor of the silverparticles AgNO3 was used. The XRD pattern of the solublePI-silver nanocomposite 6a. shows five diffraction peaks <strong>in</strong>the XRD patterns of samples 6a widen greatly, <strong>in</strong>dicat<strong>in</strong>g theformation of the nanometer scale of silver particles <strong>in</strong> the PIsilvernanocomposite. Figure 1 conta<strong>in</strong><strong>in</strong>g diffraction signalsat 2h values of 38.2 º, 45.3 º, 66.1 º, 75.5 º and 83.7 attributedto the diffraction planes (1 1 1), (2 0 0), (2 2 0), (3 1 1) and (22 2) of fcc silver nanoparticles confirm<strong>in</strong>g the presence ofsilver nanoparticles <strong>in</strong> the nanocomposites. The SEMmicrograph of the PI-silver nanocomposite 6a <strong>in</strong> figure 1shows that the silver nanoparticles were homogeneouslydispersed <strong>in</strong> polyimide matrix (Figure 1).0B[1] Lewis, L.N. Chemical Review 93: 2693-2730 (1993).[2] Huang, J.C., Qian, X.F., Y<strong>in</strong>, J., Zhu, Z.K. and Xu, H.J.Materials Chemistry and Physics 69: 172-175 (2001).[3] Rob<strong>in</strong>, E.S. and David, W.T. Chemistry Material 16: 1277-1284 (2004).[4] Hengle<strong>in</strong>, A. Chemical Review 89: 1861-1873 (1989)[5] Kobayashi, T. and Iwaki, M. Surface and Coat<strong>in</strong>gsTechnology: 196, 211-215 (2005).6th Nanoscience and Nanotechnology Conference, zmir, 2010 721
Poster Session, Thursday, June 17Theme F686 - N1123Intercalation of laurate anions <strong>in</strong>to Mg-Al layered double hydroxide:Synthesis and characterizationNathalie Gerds, †‡* Jens Risbo, † Christian B. Koch, ‡ Vimal Katiyar, § David Plackett § and Hans Christian B. Hansen ‡† Department of Food Science, Faculty of Life Sciences, Rolighedsvej 30, University of Copenhagen, DK-1958 Frederiksberg C, Denmark,‡ Department of Basic Sciences and Environment, Faculty of Life Sciences, University of Copenhagen, Thorvaldsensvej 40, DK-1871Frederiksberg C, Denmark and§ Solar Energy Programme, Risø National Laboratory for Susta<strong>in</strong>able Energy, Technical University of Denmark, 4000 Roskilde, DenmarkAbstract—Laurate anions were <strong>in</strong>tercalated <strong>in</strong>to Mg-Al layered double hydroxide (LDH) us<strong>in</strong>g coprecipitation under constant pH. Forcomparison LDH-laurate was also prepared by anion-exchange and reconstruction from calc<strong>in</strong>ed LDH. Different synthesis conditions were<strong>in</strong>vestigated show<strong>in</strong>g that a crystall<strong>in</strong>e LDH-laurate phase can be obta<strong>in</strong>ed by comb<strong>in</strong><strong>in</strong>g an Mg-Al-ratio of 2:1 with a stoichiometrical amount ofdecanoic acid and post- synthesis hydrothermal treatment at 75°C for 12h. Powder X-ray diffraction and Fourier-Transform IR-spectraconfirmed the <strong>in</strong>tercalation of the laurate anions <strong>in</strong> the <strong>in</strong>terlayer. From the TEM and SEM micrographs it can be seen that the particlemorphology has a nanoporous structure conta<strong>in</strong><strong>in</strong>g <strong>in</strong>terconnected platelets with a particle size <strong>in</strong> the range of 100-250 nm. Our work showedthat LDH-laurate can be prepared by coprecipitation with comparable characteristics to that of the compound produced us<strong>in</strong>g the ion-exchangemethod.Intercalation of organic anions <strong>in</strong>to layered double hydroxides(LDHs) is required for the successful development ofpolymer–LDH nanocomposites. Surfactant-<strong>in</strong>tercalated LDHhave been commonly used as nanofillers <strong>in</strong> polymers ow<strong>in</strong>g totheir nanoscale structure and excellent enhancement ofphysical (e.g., barrier) and chemical properties [1].Furthermore, LDHs can be used <strong>in</strong> controlled release drugdelivery systems and removal of organic pollutants from soiland water [2-3]. Intercalation of long-cha<strong>in</strong> anion surfactant<strong>in</strong>to the LDH is an attractive way to make the <strong>in</strong>terlayer spaceacceptable for polymers. The modification of the host materialresults <strong>in</strong> hydrophobic surface character of the layercompound and yields an extension of the <strong>in</strong>terlayer distance.There are relatively few reports on the <strong>in</strong>tercalation of longcha<strong>in</strong>carboxylates <strong>in</strong>to LDH us<strong>in</strong>g coprecipitation methods.Most of the published LDH <strong>in</strong>vestigations us<strong>in</strong>g acoprecipitation method were conducted with organic anionsconta<strong>in</strong><strong>in</strong>g sulfonates [4-5]. The objective of this work was tocreate a fast, cost effective and environmentally friendlypreparation method us<strong>in</strong>g long-cha<strong>in</strong> carboxylates. In ourresearch decanoate (laurate) anions have been <strong>in</strong>tercalated <strong>in</strong>toMg-Al-LDH by coprecipitation <strong>in</strong> the presence of an ethanoliclaurate solution kept at constant pH.In our study, we showed that the direct synthesis can result <strong>in</strong>a multi-phase system. X-ray diffraction analysis identified thepresence of two series of basal reflection peaks demonstrat<strong>in</strong>gthat two layered compounds were formed. Hence, <strong>in</strong> order todist<strong>in</strong>guish the LDH-laurate phases and the by-products,laurate-<strong>in</strong>tercalated Mg-Al-LDH was prepared by the ionexchangeand reconstruction method and used as referencematerial. Furthermore, the <strong>in</strong>fluence of the Mg-Al-ratio of 2:1and 3:1 was <strong>in</strong>vestigated.It was found that the solvent system, the Mg:Al ratio and theconcentration of the carboxylic acid are critical parameters <strong>in</strong>the direct synthesis. An Mg-Al-ratio of 2:1 causes theformation of the <strong>in</strong>tercalated LDH-laurate phase whereas anMg-Al-ratio of 3:1 and excess of laurate anions favours theformation of Mg-laurate as a co-exist<strong>in</strong>g secondary phase. Apure crystall<strong>in</strong>e LDH-laurate phase was obta<strong>in</strong>ed bycomb<strong>in</strong><strong>in</strong>g an Mg-Al-ratio of 2:1 with a stoichiometricalamount of decanoic acid and post-synthesis hydrothermaltreatment at 75°C for 12h. The powder X-ray-diffractionpattern of the laurate-<strong>in</strong>tercalated LDHs prepared by thedifferent synthesis routes shows that the <strong>in</strong>tercalated form hasa hydrotalcite-like structure.a) b)Figure 1: a) Scann<strong>in</strong>g electron micrograph and b) transmission electronmicroscope images from an LDH-laurate sample prepared by the directsynthesis.The observed basal spac<strong>in</strong>gs are almost the same regardless ofthe synthesic route. This suggests that the laurate anions are<strong>in</strong>tercalated as a monolayer <strong>in</strong> which the carboxylate cha<strong>in</strong>s lieperpendicular to the brucite-like layers. Fourier-Transform IRspectraconfirmed the <strong>in</strong>tercalation of the laurate anions <strong>in</strong> the<strong>in</strong>terlayer. Transmission electron microscopy (TEM) andscann<strong>in</strong>g electron microscopy (SEM) were used to study thecrystal morphology structure. Typically, the different samplesshow similar plate–like morphology with particle sizes <strong>in</strong> therange of 100-250 nm. The direct synthesis results <strong>in</strong> ananoporous structure consist<strong>in</strong>g of <strong>in</strong>terconnected platelets asseen <strong>in</strong> Figure 1a-b. This work is part of the current NanoPackproject (http://www.nanopack.dk) funded by the DanishStrategic Research Council.*Correspond<strong>in</strong>g author: ng@life.ku.dk[1] H.B. Hsueh and C.Y. Chen. Polymer 44, 5275 (2003).[2] Y.W. You et al., Colloids Surf. A: Physicochem. Eng. Aspects 205,161 (2002).[3] B.X. Li et al., Int. J. Pharm. 287, 89 (2004).[4] B. Wang et al., Mater. Chem. Phys. 92 190 (2005).[5] H. Zhang et al., J. Solid State Chem. 180, 1636 (2007).6th Nanoscience and Nanotechnology Conference, zmir, 2010 722
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