Poster Session, Thursday, June 17Theme F686 - N1123Fabrication of Plat<strong>in</strong>um Nanoparticles Us<strong>in</strong>g Amphiphilic Copolymer TemplateNuman HODA*, Burç<strong>in</strong> ACAR, Leyla BUDAMA, Önder TOPELAkdeniz University Department of Chemistry Antalya TurkeyAbstract-Production of nanoparticles with controlled size is important for their properties. In this study, production of Ptnanoparticles us<strong>in</strong>g PB-b-PEO amphiphilic copolymer template to control their size by load<strong>in</strong>g different amount of precursor was tried.Synthesis of nanoparticles of metals, semiconductorsand magnetic <strong>crystals</strong> has been accomplished by severalmethods <strong>in</strong>clud<strong>in</strong>g amphiphilic copolymer template. Thesek<strong>in</strong>ds of copolymers have ability to form micelles <strong>in</strong> dilutesolutions <strong>in</strong> selective solvents for one of the blocks [1].Metal salts can be encapsulated <strong>in</strong> the core of micelles bycomplexation or association, corona provides stabilization.Encapsulated metals are easily chemically reduced oroxidized to convert them their nanoparticles.The aim of study is to control Pt nanoparticles size byadd<strong>in</strong>g different amount of precursor to copolymermicelles.PB-b-PEO is a typical amphiphilic copolymer whichcan form micelle <strong>in</strong> aqueous solution. In characterizationof copolymer PB1800-b-PEO4000 (from Polymer Sources,Canada) micelles formed <strong>in</strong> aqueous solution,hydrodynamic diameter of micelles (D h ) was found to be52.4(±2) nm. DLS method also gives <strong>in</strong>formation aboutpolydispersity of the micelles and this was about 0.075.The cmc of PB-b-PEO diblock copolymer <strong>in</strong> aqueoussolution was estimated to be 2.94x10 -7 M by fluorescencespectroscopy.PB-b-PEO diblock copolymer micelles <strong>in</strong> aqueoussolution were used to as nanoreactor to produce Ptnanoparticles hav<strong>in</strong>g certa<strong>in</strong> sizes. To control particle sizeamount of salt to be added was changed. TEM Picture wastaken <strong>in</strong> 120 kV. The PB-b-PEO diblock copolymermicelles from TEM are showed <strong>in</strong> Fig. 1. Result<strong>in</strong>gpictures with different metal:polymer ratio (<strong>in</strong> mol) aregiven <strong>in</strong> Figs. 2.a-f with the size distribution.Figure 1. Micelles of PB-b-PEO <strong>in</strong> aqueous solutionFigure 2. Nanoparticles produced <strong>in</strong> a;(3:1) , b;(1:1), c;(1:5),d;(1:10), e;(1:15), f;(1:20), metal:polymer load<strong>in</strong>g.When metal:polymer ratio is favor of metal for example, 3:1,micelles do not stabilize all of metal salt added accord<strong>in</strong>g toFig.2a. In this figure, there are some agglomerates outside ofthe micelle. It may be understood that the complexationbetween metal salt and hydrophobic part of the copolymer isweak. It can be seen that <strong>in</strong> the other pictures nanoparticlesare dispersed homogeneously. The mean diameters ofnanoparticles for 1:1, 1:5, 1:10 and 1:20 ratios are 1.3(2),1.5(3), 1.4(3) and 1.1(2) nm, respectively. Accord<strong>in</strong>g toTEM pictures of nanoparticles obta<strong>in</strong>ed <strong>in</strong>creas<strong>in</strong>g amount ofmetal salt load<strong>in</strong>g to micelles does not affect much the sizeof nanoparticles. This work was supported by AkdenizUniversity the Scientific Research Projects Coord<strong>in</strong>ationUnit under Grant No. 2007.01.0105.007.*Correspond<strong>in</strong>g Author: nhoda@akdeniz.edu.tr[1] G. Riess, Prog. Polym. Sci., 2003, 28, 1107.6th Nanoscience and Nanotechnology Conference, zmir, 2010 654
PPoster Session, Thursday, June 17Theme F686 - N1123Alternative Method to Production of Nano-Sized -SiAlON Powders111Onur EserP P, USemra KuramaUP P* and Göktug GünkayaP1PDepartment of Materials Science and Eng<strong>in</strong>eer<strong>in</strong>g, Anadolu University, Eskisehir, TurkeyAbstract-In this study, the optimum mill<strong>in</strong>g system was <strong>in</strong>vestigated by us<strong>in</strong>g sedimentation method. The effect of type of mediums anddispersants were researched by us<strong>in</strong>g sedimentation tests. After the optimization of mill<strong>in</strong>g medium wet mill<strong>in</strong>g system was used to decreas<strong>in</strong>gparticle size of start<strong>in</strong>g powders. All the mill<strong>in</strong>g time results were discussed related with the particle size of milled powder.There are some routes to prepare nano-sized SiAlONpowders such as plasma-chemical and laser synthesis [1], solgeland as a top-to-bottom process high-energy mechanicalmill<strong>in</strong>g [2]. Although, this method promises very low particlesizes (~40 nm), would <strong>in</strong>crease the cost of the <strong>in</strong>itial powder[3]. In this study -SiAlON described as SiR4RAlR2ROR2RNR6R, anddoped with 5 wt.% YR2ROR3R. The weighed powders wereplanetary ball milled (Pulverisette 6 Fritsch, Germany) withSiR3RNR4R balls for 2 h <strong>in</strong> different solvent compositions (toluene,methyl ethyl keton, ethanol) and <strong>in</strong> different ratios. Thesolvent ratios were determ<strong>in</strong>ed as given <strong>in</strong> the literature [4].The level of agglomeration, a critical parameter for theefficiency of the mill<strong>in</strong>g process, was determ<strong>in</strong>ed us<strong>in</strong>g thesedimentation method. As expla<strong>in</strong>ed <strong>in</strong> our previous study [5],the most dispersed solvent composition was determ<strong>in</strong>ed for-SiAlON system <strong>in</strong> three k<strong>in</strong>ds of dispersant (oleic acid,polyethyleneglicol, sodium tripolyphosphate). In the presentstudy polyv<strong>in</strong>ylpyrrolidon was also <strong>in</strong>vestigated as analternative to the other three <strong>in</strong> the -SiAlON system. Theoptimum solvent ratio was <strong>in</strong>vestigated <strong>in</strong> an ethanol:toluenesystem of 70:30 vol. ratio with the highest sedimentationheight. The effect of the dispersant <strong>in</strong> the selected solventcomposition was <strong>in</strong>vestigated by addition of oleicacid, STPP(sodium tripolyphosphate), PEG (polyethyleneglicol) and PVP(polyv<strong>in</strong>ylpyrrolidon) as dispersants (Figure 1).Sediment height (mm)130125120115110105100950 0.5 1 1.5 2 2.5 3PVP(wt. %)Time (h)Figure 1. Effect of amount of (a) PVP on sedimentation heightAccord<strong>in</strong>g to the result, the b<strong>in</strong>ary solvent system of ethanoland toluene (at a volume ratio 70:30) with 3 wt.% addition ofPVP shows the most dispersed behavior and is used as amill<strong>in</strong>g medium for mill<strong>in</strong>g studies. The first powder producedby conventional method which has a powder:ball:alcohol ratioof 1:1.5:2 and the other powder produced by high-energymechanical mill<strong>in</strong>g <strong>in</strong> wet medium at 450 rpm for differenttimes up to 40 hours. For the characterization of the particlesize of the milled powders, two different types of method wereused <strong>in</strong> this study. One of these is the dynamic light scatter<strong>in</strong>gmethod, and the average particle size of the milled powders isgiven <strong>in</strong> Fig. 2-3.The second method, BET, was used tomeasure the surface area of the powders an the mean particlesize of (DRBETR). Comparison of the results of both methodsshows that even though the particle size of powders decrease0.51.02.52.01.53.0by <strong>in</strong>creas<strong>in</strong>g mill<strong>in</strong>g time, from sample C to N50. There wasobserved differences <strong>in</strong> results. These differences can beexpla<strong>in</strong>ed by the formation of agglomerates which are difficultto deform, even us<strong>in</strong>g ultrasonic treatment <strong>in</strong> the dynamic lightscatter<strong>in</strong>g method. However, <strong>in</strong> the BET method the diffusionof NR2R gas <strong>in</strong>to agglomerates is possible, giv<strong>in</strong>g more realisticresults than the dynamic light scatter<strong>in</strong>g method.Particle Size (nm)7006005004003002001000Conventional51020Time (h)Figure 2. Particle size analyse of powder by dynamic light scatter<strong>in</strong>gmethodParticle Size (nm)250200150100500Conventional51020Time (h)Figure 3. Particle size analyse of powder by BETAs a consequence, the high energy mill<strong>in</strong>g <strong>in</strong> a wet mediumsystem is an effective way to produce nano- -SiAlONstart<strong>in</strong>g powders. The most efficient mill<strong>in</strong>g medium for the-SiAlON suspensions is <strong>in</strong>vestigated as 70 vol. % Ethanol-30vol. % Toluen with the addition of 3 wt% PVP. The m<strong>in</strong>imum-SiAlON powder size was obta<strong>in</strong>ed as 92 nm after 50 hmill<strong>in</strong>g <strong>in</strong> this medium.This work was supported by TUBITAK under Grant No.108T661.*Correspond<strong>in</strong>g author: skurama@anadolu.edu.tr[1]. Bulic, F., Zalite, I., Zhil<strong>in</strong>ska, N., 2004. Comparison of plasma-chemicalsynthesised SiAlON nano-powder and conventional prepared SiAlONpowder, Journal of the European Ceramic Society, 24: 3303-3306.[2]. Li, Q., Zhang, C., Komeya, K., Tatami, J., Meguro, T., Gao, L., 2003.Nano powders of -SiAlON carbothermally produced via a sol-gel process,Journal of Materials Science Letters, 22: 885-887.[3]. Xu, X., Nishimura, T., Hirosaki, N., Xie, R., Yamamoto, Y., Tanaka, H.,2005. Fabrication of -SiAlON nanoceramics by high-energy mechanicalmill<strong>in</strong>g and spark plasma s<strong>in</strong>ter<strong>in</strong>g, Nanotechnology, 16 : 1569-1573.[4] Eser, O. and Kurama, S., (2010). The effect of the wet-mill<strong>in</strong>g process ons<strong>in</strong>ter<strong>in</strong>g temperature and the amount of additive of SiAlON ceramics,Ceramics International, doi:10.1016/j.ceram<strong>in</strong>t.2009.12.025.[5] Eser, O., Kurama, S. and Gunkaya, G., 2010. The production of -SiAlON ceramics with low amount of additive, at low s<strong>in</strong>ter<strong>in</strong>g temperature,J. The European ceram. Soc,. doi: 10.1016/j.jeurceramsoc.2010.01.024.3030404050506th Nanoscience and Nanotechnology Conference, zmir, 2010 655
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