PPP HR3RBOR3Poster Session, Thursday, June 17Theme F686 - N1123Performance of Z<strong>in</strong>c Borate Nanoparticles as an Anti-Wear Additive <strong>in</strong> M<strong>in</strong>eral Oil1211USevdiye Atakul SavrkUP P*, Mehmet GönenP P, Devrim BalköseP P, Semra ÜlküP1Pzmir Institute of Technology, Department of Chemical Eng<strong>in</strong>eer<strong>in</strong>g, Gülbahçe Köyü, Urla, zmir, Turkey2PPresent address: Süleyman Demirel University, Department of Chemical Eng<strong>in</strong>eer<strong>in</strong>g, Isparta, TurkeyAbstract- Inorganic borates as a lubricat<strong>in</strong>g oil additive received extensive attention <strong>in</strong> recent years due to the remarkable tribologicalproperties such as wear resistance, friction-reduc<strong>in</strong>g ability and oxidation <strong>in</strong>hibition. This study reports the synthesis of nano-sized z<strong>in</strong>c borate,its characterization as well as its performance <strong>in</strong> m<strong>in</strong>eral oil as a lubricat<strong>in</strong>g additive. Z<strong>in</strong>c borate nanoparticles with different morphologieswere prepared by two different raw materials groups. Spherical <strong>crystals</strong> were successfully synthesized by precipitation reaction <strong>in</strong> aqueoussolutions of NaR2RBR4ROR7R·10HR2RO and ZnNR2ROR6R·6HR2RO, whereas supercritical ethanol dry<strong>in</strong>g method is applied to prepare broccoli type speciesafter the precipitation step <strong>in</strong> aqueous solutions of HR3RBOR3R and ZnO. The lubricants were prepared by dispers<strong>in</strong>g the z<strong>in</strong>c borate particles withsorbitan monostearate (Span 60) which was used as a surface modifier. The tribological properties of the m<strong>in</strong>eral oil were determ<strong>in</strong>ed by fourballwear test mach<strong>in</strong>e and the results <strong>in</strong>dicated that wear scar diameter is reduced by 54.78% for the lubricant <strong>in</strong>clud<strong>in</strong>g z<strong>in</strong>c borate dried bysupercritical ethanol dry<strong>in</strong>g compared to that of the m<strong>in</strong>eral oil.The <strong>in</strong>creas<strong>in</strong>g <strong>in</strong>terest of petrochemical <strong>in</strong>dustries onimprov<strong>in</strong>g the performance of their products (lubricants,greases, gasol<strong>in</strong>e, among others) has been simultaneouslygenerat<strong>in</strong>g great <strong>in</strong>centives to develop additives that are ableto supply the commercial demand of the competitive <strong>in</strong>dustrialmarkets. For tribology applications, particles as additives <strong>in</strong>base oil have been <strong>in</strong>vestigated widespreadly. These studiesrefer to synthesis and preparation of especially nanoscaleparticles, and their tribological properties and mechanisms[1,2]. The lubrication performance of a lubricant relies partlyupon the thickness of the tribofilm under the severe conditionscontrolled by several parameters such as load, temperature,slid<strong>in</strong>g speed and the mechanical properties of the film. Avariety of mechanisms have been proposed to expla<strong>in</strong> thelubrication enhancement of the nanoparticles suspended <strong>in</strong>lubricat<strong>in</strong>g oil. Ball bear<strong>in</strong>g effect and protective filmmechanisms have direct effect of the nanoparticles onlubrication enhancement, whereas mend<strong>in</strong>g and polish<strong>in</strong>geffects have secondary effect on surface improvement [3].This study aims to <strong>in</strong>vestigate the tribological properties ofm<strong>in</strong>eral oil <strong>in</strong>clud<strong>in</strong>g z<strong>in</strong>c borate nanoparticles and to exposethe effect of morphology of the particles on anti-wearproperty.In this project, first group of z<strong>in</strong>c borate species wereobta<strong>in</strong>ed by the homogenous precipitation method describedby T<strong>in</strong>g et al. us<strong>in</strong>g ZnNR2ROR6R·6HR2RO, NaR2RBR4ROR7R·10HR2RO andammonia [4]. Second group of z<strong>in</strong>c borate nanoparticles were3prepared by 4.7mol/dmPRwith the stoichiometricamount of ZnO. Supercritical ethanol dry<strong>in</strong>g of submicronz<strong>in</strong>c borate was performed at 250 °C, 6.5 MPa for obta<strong>in</strong><strong>in</strong>gnano z<strong>in</strong>c borate particles. All z<strong>in</strong>c borate samples werecharacterized by SEM, TGA, DSC, FTIR, and XRD. Thelubricants were prepared by add<strong>in</strong>g sorbitan monostearate(Sigma Aldrich) and z<strong>in</strong>c borate particles <strong>in</strong>to the m<strong>in</strong>eral oilat 70 °C. They were mixed by both a homogenizer (OMNIGLH) and a magnetic stirrer (Yellowl<strong>in</strong>e MSH Basic) for 2m<strong>in</strong>utes and 2 hours, respectively. Tribologicalcharacterization of the lubricants was carried out by a fourballwear test mach<strong>in</strong>e (made by Falex Corp.) The test ballswere chrome alloy steel, No. E-52100 with a diameter of 12.7mm. The wear and friction test was performed at 392 N andthe test duration was 1h. After the test, the morphology ofworn surfaces of the balls run <strong>in</strong> the lubricant was obta<strong>in</strong>ed bySEM. Moreover, elemental composition of the ball wornsurfaces was determ<strong>in</strong>ed by EDX analysis.SEM images of z<strong>in</strong>c borate nanoparticles produced bydifferent raw materials groups are shown <strong>in</strong> Figure 1. Thez<strong>in</strong>c borate obta<strong>in</strong>ed by ZnNR2ROR6R·6HR2RO andNaR2RBR4ROR7R·10HR2RO <strong>in</strong>cludes spherical <strong>crystals</strong> (Figure 1a). Onthe other hand, z<strong>in</strong>c borate <strong>crystals</strong> dried by supercriticalethanol have broccoli type morphologies. Table 1 reports thetribological properties of the lubricants. It was revealed thatsorbitan monostearate had a dramatic role <strong>in</strong> the reduction ofwear scar diameter from 1.402 to 0.656 mm. When thenanoparticles dried by supercritical ethanol were used aslubricat<strong>in</strong>g oil additives, wear scar diameter is reduced to0.634 mm.(a)(b)Figure 1. SEM images of super critical ethanol dried nanoparticlesobta<strong>in</strong>ed from z<strong>in</strong>c borates a) ZnNR2ROR6R·6HR2RO and NaR2RBR4ROR7R·10HR2ROand b)HR3RBOR3R and ZnOTable 1. Tribological properties of lubricantsWear Scar FrictionSample AdditiveDiameter (mm) CoefficientL1 - 1.402 1.645L2 Span 60 0.656 1.635L3ZB dried bySCE +Span 600.634 1.601SEM analysis shows that the worn surface of the balllubricated with L3 lubricant <strong>in</strong>clud<strong>in</strong>g z<strong>in</strong>c borate andsurfactant exhibits much smoother surfaces without severescuff<strong>in</strong>g. Additionally, EDX analysis reveals that boron andz<strong>in</strong>c elements are also adsorbed by the worn surface of theball.TÜBTAK (project number: 105M358), OPET PetrolcülükA. and Izmir Institute of Technology Centre for MaterialResearch are greatly appreciated.HT*Correspond<strong>in</strong>g author: sevdiyeatakul@iyte.edu.trT[1] Zhang M., Wang X., Fu X., Xia Y., 2009. Performance andanti-wear mechanism of CaCOR3 Rnanoparticles as a green additive <strong>in</strong>poly-alpha-olef<strong>in</strong>, Tribology International, 42:1029-1039.[2] Choundary R.B., Pande P.P., 2006. Lubrication potential ofboron compounds: an overview. Lubrication Science, 14: 211-222.[3] Lee K., Hwang Y., Cheong S., Choi Y., Kwon L., Lee J., KimS.H., 2009. Understand<strong>in</strong>g the role of nanoparticles <strong>in</strong> Nano-oillubrication, Tribology Letters, 35: 127-131.[4] T<strong>in</strong>g C., Cheng D.J., Shuo W.L., Gang F., 2009. Preparationand characterization of nano-z<strong>in</strong>c borate by a new method, Journalof Material Process<strong>in</strong>g Technology, 209:4076-4079.6th Nanoscience and Nanotechnology Conference, zmir, 2010 733
andPCPPoster Session, Thursday, June 17Preparation and Characterization of Poly (3-Hydroxybutyrate) Homo and CopolymersNanocomposite Films1111Onur GökbulutP P, Burcu KayaP P, Okan AknP Pand UFunda Tihm<strong>in</strong>liogluUP P*1PDepartment of Chemical Eng<strong>in</strong>eer<strong>in</strong>g, zmir Institute of Technology, Urla, 35430, TurkeyTheme F686 - N1123Abstract- This study aims to prepare and <strong>in</strong>vestigate the characteristic properties of Poly (hydroxybutyrate) (PHB) andpolyhydroxybutyrate-co valerate (PHB/HV) copolymers layered silicate nanocomposites. Nanocomposites were prepared via melt<strong>in</strong>tercalation method by dispers<strong>in</strong>g orgonamodified layered silicate nanoclays. The effects of clay load<strong>in</strong>g and the polymer type on the watervapour, OR2R COR2R barrier properties were measured. In addition, Differential Scann<strong>in</strong>g Calorimetry (DSC) and mechanical properties ofthe films were performed. Mechanical properties of the chitosan composites were enhanced with the addition of clay . The enhancement <strong>in</strong>the barrier properties were obta<strong>in</strong>ed upto certa<strong>in</strong> clay content <strong>in</strong> composites.Among many different materials that mank<strong>in</strong>d is dependenton plastics are the most important ones consider<strong>in</strong>g theirwidespread usage <strong>in</strong> food packag<strong>in</strong>g, textile, communication,transportation, construction, medical <strong>in</strong>dustries. Currently,plastics and synthetic polymers are ma<strong>in</strong>ly produced us<strong>in</strong>gpetrochemical materials that cannot be decomposed. Inaddition the amount of plastic waste <strong>in</strong>creases every year.Therefore <strong>in</strong> the last decades there has been a significant<strong>in</strong>crease <strong>in</strong> the development of biodegradable thermoplasticpolyesters due to ongo<strong>in</strong>g concerns about the disposal ofconventional plastics and the <strong>in</strong>creas<strong>in</strong>g difficulty <strong>in</strong>manag<strong>in</strong>g solid wastes.Poly (hydroxyalkanoates), PHAs, comprise a family ofbiopolymers that has attracted much attention recently due tosimilar properties to conventional materials such aspolypropylene, polyethylene, polystyrene, and PET. Bacterialbiopolymers such as Poly (3-hydroxybutyrate) (PHB) and itscopolymers with valerate (PHB/HV) are biodegradablethermoplastic polyesters and one of the most widely<strong>in</strong>vestigated members of the family of PHAs. PHB and itscopolymers present good mechanical, thermal and barrierproperties. PHB is a partially crystall<strong>in</strong>e thermoplastic andhas a high melt<strong>in</strong>g temperature. However PHB suffers fromlow melt<strong>in</strong>g stability, brittleness and lack of transparency [1].Thus, recent studies are objected to improve the properties ofPHB and its copolymers by addition of nanoclays. Surfacemodified clays have been studied as advanced additives toimprove or balance thermal, mechanical, fire resistance,surface, or conductivity properties of nanocomposite due totheir high surface to volume ratios and the subsequent<strong>in</strong>timate contact that they promote with the matrix at lowfiller additions [2]. In essence, three different methods areused to synthesize polymer-clay nanocomposite; melt<strong>in</strong>tercalation, solution and situ polymerization.PHB and PHB-HV /layered silicate nanocomposites <strong>in</strong> thepresent study are prepared via melt extrusion. Natural PHBand its copolymer PHB-HV (2% and 12%) were purchasedfrom Goodfellow Inc. and dried under vacuum at 80°C fortwo days before use. As clay, organophilic surface modifiedmontmorillonite called Cloisite® 15A purchased fromSouthern Clay Products, Inc. Polymers and nanoclay aremelted extruded by us<strong>in</strong>g a Thermofisher tw<strong>in</strong> screw extruderwith vary<strong>in</strong>g weight percentages of clay at a temperature of180 °C and a screw speed of 50 rpm. The extrudedcomposites are dried under vacuum at 50 °C. The samples ofPHB, PHB-HV and their nanocomposite are f<strong>in</strong>allytransformed <strong>in</strong>to films by compression mold<strong>in</strong>g <strong>in</strong> a hot-plateohydraulic press at 175 P PC and 5 Metric tons of pressuredur<strong>in</strong>g 5 m<strong>in</strong>. The polymer sheets are cooed to roomtemperature under constant pressure.The effect of filler concentration on the water vapor, OR2Rand COR2 Rpermeability, mechanical and thermal properties ofthe composite films were evaluated. The structure ofnanocomposites and the state of <strong>in</strong>tercalation of the clay werecharacterized by Phillips X’Pert Pro MRD with Cu Kradiation (=1.54 nm) under a voltage of 40 kV and a currentof 40 mA. Samples were scanned over the range ofdiffraction angle 2 = 0.25-30°. Thermal properties of thepolymer and the nanocomposite films are studied by a DSCtechnique with a Shimadzu Calorimeter at a heat<strong>in</strong>g rate 10oP/m<strong>in</strong>. Morphology of polymers and their nano compositesare analyzed by XRD and TEM. As a result of morphogicalanalyses , <strong>in</strong>tercalated structure were obta<strong>in</strong>ed . The extent of<strong>in</strong>tercalation depends on the amount of silicate and the natureof organic modifier present <strong>in</strong> the layered silicate .Accord<strong>in</strong>g to results of permeability measurements; thenanocomposite films exhibit good barrier properties ascompared to their unfilled polymer films. The water vaporand gas permeability values of the composite films decreasedsignificantly depend<strong>in</strong>g on the filler concentration and thetype of filler used. The decrease <strong>in</strong> water vapor and gaspermeability of PHB and PHB-HV- clay nanocompositefilms are believed to be due to the presence of ordereddispersed clay nanoparticle layers with large aspect ratios <strong>in</strong>the polymer matrix. This causes an <strong>in</strong>crease <strong>in</strong> effective pathlength for diffusion of water vapour and gas <strong>in</strong>to polymermatrix.*Correspond<strong>in</strong>g author: HTfundatihm<strong>in</strong>lioglu@iyte.edu.trT[1] M. D. Sanchez-Garcia ; E. Gimenez ; J. M. Lagaron ,Morphology and Barrier Properties of Nanobiocomposites ofPoly(3-hydroxybutyrate) and Layered Silicates Wiley InterScience2008 , DOI 10.1002/app.27622[2] Reguera, J.; Lagaron, J. M.; Alonso, M.; Reboto, V.; Calvo, B.;Rodriguez-Cabello, J. C. Macromolecules 2003, 36, 8470.[3] Cabedo L.; Plackett D.;Gimenez E.; Lagaron J.M., Study<strong>in</strong>g theDegradation of Polyhydroxybutyrate-covalerate dur<strong>in</strong>g Process<strong>in</strong>gwith Clay-Based Nanofillers Received 31 March 2008; accepted 22September 2009, DOI 10.1002/app.29945[4] Pralay Maiti, Carl A. Batt, and Emmanuel P. Giannelis, NewBiodegradable Polyhydroxybutyrate/Layered SilicateNanocomposites , Biomacromolecules 2007, 8, 3393-34006th Nanoscience and Nanotechnology Conference, zmir, 2010 734
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